γ-Ray spectrometry of radon in water and the role of radon to representatively sample aquifers

International Nuclear Information System (INIS)

Talha, S.A.; Lindsay, R.; Newman, R.T.; Meijer, R.J. de; Maleka, P.P.; Hlatshwayo, I.N.; Mlwilo, N.A.; Mohanty, A.K.

2008-01-01

Measurement of radon in water by γ-ray spectrometry using a HPGe detector has been investigated to determine aquifer characteristics. The radon activity concentration is determined by taking the weighted average of the concentrations derived from γ-ray lines associated with 214 Pb and 214 Bi decay. The role of accurate radon data to representatively sample aquifers was also investigated by studying a semi-cased borehole. A simplified physical model describing the change of radon concentration with the pumping time, reproduces the data and predicts the time for representative sampling of the aquifer

Aircraft gamma-ray spectrometry in snow-water equivalent measurement

Energy Technology Data Exchange (ETDEWEB)

Kuittinen, R; Vironmaeki, J

1979-01-01

During the winter periods of 1976 to 1977 and 1977 to 1978, the Hydrological Office at the National Boards of Waters and the Geological Survey of Finland carried out a joint study to evaluate usefulness of gamma-ray spectrometry in snowwater equivalent measurement. A multichannel gamma-ray spectrometry was fitted out in a DC-3 aircraft. Fourteen snow courses were operated using gravimetric method and gamma-ray method. The snow courses were located in southern Finland in forest, swamp and agricultural land. The results show that the gamma ray method can be considered suitable for use in Finnish conditions and the accuracy of the gamma-ray method is almost of the same magnitude of the accuracy of the gravimetric method.

Accurate isotope ratio mass spectrometry. Some problems and possibilities

International Nuclear Information System (INIS)

Bievre, P. de

1978-01-01

The review includes reference to 190 papers, mainly published during the last 10 years. It covers the following: important factors in accurate isotope ratio measurements (precision and accuracy of isotope ratio measurements -exemplified by determinations of 235 U/ 238 U and of other elements including 239 Pu/ 240 Pu; isotope fractionation -exemplified by curves for Rb, U); applications (atomic weights); the Oklo natural nuclear reactor (discovered by UF 6 mass spectrometry at Pierrelatte); nuclear and other constants; isotope ratio measurements in nuclear geology and isotope cosmology - accurate age determination; isotope ratio measurements on very small samples - archaeometry; isotope dilution; miscellaneous applications; and future prospects. (U.K.)

Measurements of uranium enrichment by four techniques of gamma-ray spectrometry

International Nuclear Information System (INIS)

Tojo, Takao

1983-12-01

Measurements of uranium enrichment with the uses of the LMRI (France) UO 2 standards have been made by four techniques of gamma-ray spectrometry, in order to examine measurement characteristics of each technique. The following results were obtained by the three techniques based on the direct determination of the peak area of the 186-keV gamma-rays from 235 U, when the standard sample of 6.297 a/o was used for measuring enrichments ranging from 1.4 a/o to 9.6 a/o ; (i) In a LEPS HP Ge gamma-ray spectrometry, standard deviation of the measured enrichments from the certified ones was 1.4 %, (ii) in a Ge(Li) gamma-ray spectrometry, the standard deviation was 2.0 %, (iii) in a NaI(Tl) gamma-ray spectrometry, the standard deviation was 1.2 %. In the fourth technique, the method of multiple single-channel analyzers, enrichments of 1.4 - 9.6 a/o were measured in the standard deviation of 0.51 %, when the most suitable pairs of standard samples were used for each sample. A part of sources of systematic errors which were caused by each technique adopted was revealed throughout the measurements. And also, it was recognized that the LMRI's values of enrichment were certified precisely, and the UO 2 standards were very useful for enrichment measurements in the four techniques of gamma-ray spectrometry used here. (author)

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

Detector calibration for in-situ gamma ray spectrometry

CERN Document Server

Balea, G

2002-01-01

The power in the technique of in-situ spectrometry lies in the fact that a detector placed on ground measures gamma radiation from sources situated over an area of several hundred square meters. The 'field of view' for the detector would be larger for high energy radiation sources and for sources closer to the soil surface. In contrast, a soil sample would represent an area of a few tens of hundreds of square centimeters. In practice, an effective characterization of a site would involve in-situ gamma ray spectrometry in conjunction with soil sampling. As part of an overall program, in-situ gamma ray spectrometry provides a means to assess the degree of contamination in areas during the course of operations in the field, thus guiding the investigator on where to collect samples. It can also substantially reduce the number of samples need to be collected and subsequently analyzed. (author)

Advances in continuous gamma-ray spectrometry and applications

International Nuclear Information System (INIS)

Gold, R.; McNeece, J.P.; Kaiser, B.J.

1984-07-01

Recent advances and applications in continuous Compton recoil gamma-ray spectrometry are described. Applications of continuous gamma-ray spectrometry are presented for: (1) Characterization of light water reactor (LWR) pressures vessel (PV) environments. (2) Assessment of fuel distributions for Three Mile Island Unit 2 (TMI-2) reactor recovery. (3) Measurement of LWR-PV-neutron exposure. The latest improvements attained with the Janus probe, a special in-situ configuration of Si(Li) detectors, are presented. The status of current efforts to extend the domain of applicability of this method beyond 3 MeV is discussed with emphasis on recent work carried out with Si(Li) detectors of much larger volume

On response operator in semiconductor gamma ray spectrometry

Energy Technology Data Exchange (ETDEWEB)

Krnac, S [Slovak Technical Univ., Bratislava (Slovakia); Povinec, P [International Atomic Energy Agency, Monaco (Monaco). MEL; Ragan, R [Inst. of Preventive and Clinical Medicine, Bratislava (Slovakia)

1996-12-31

Some results of the scaling confirmation factor analysis (SCFA) application in semiconductor gamma-ray spectrometry presented in this contribution points out to a new ground for evaluation the gamma-ray spectra. This whole-spectrum processing approach considerably increases detection sensitivity, especially, if significant interferences being present in the measured spectrum. Precision of the SCFA method is determined by choice of a sufficient number of suitable calibration gamma-ray sources in the energy region of interest, by setting up an acceptable latent hypothesis and by chosen experimental quantification of spectra. The SCFA method is very advantageous to use, for instance, in ultra low-level gamma-spectrometry where counting rates in full energy peaks are extremely low as compared with background interferences. It enables to increase of the sensitivity by the 5-10 times in comparison with the traditional full energy peak net area method (J.K.). 1 fig., 2 tabs., 6 refs.

On response operator in semiconductor gamma ray spectrometry

International Nuclear Information System (INIS)

Krnac, S.; Povinec, P.

1995-01-01

Some results of the scaling confirmation factor analysis (SCFA) application in semiconductor gamma-ray spectrometry presented in this contribution points out to a new ground for evaluation the gamma-ray spectra. This whole-spectrum processing approach considerably increases detection sensitivity, especially, if significant interferences being present in the measured spectrum. Precision of the SCFA method is determined by choice of a sufficient number of suitable calibration gamma-ray sources in the energy region of interest, by setting up an acceptable latent hypothesis and by chosen experimental quantification of spectra. The SCFA method is very advantageous to use, for instance, in ultra low-level gamma-spectrometry where counting rates in full energy peaks are extremely low as compared with background interferences. It enables to increase of the sensitivity by the 5-10 times in comparison with the traditional full energy peak net area method (J.K.). 1 fig., 2 tabs., 6 refs

Portable gamma-ray spectrometers and spectrometry systems

International Nuclear Information System (INIS)

Shebell, P.

1999-01-01

The current state-of-the-art in portable gamma-ray spectrometers and portable spectrometry systems is discussed. A comparison of detector performance and features of commercially available systems are summarised. Finally, several applications of portable systems are described. (author)

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

Some deficiencies and solutions in gamma ray spectrometry

International Nuclear Information System (INIS)

Westmeier, W.

1998-01-01

A number of problems in high-resolution gamma ray spectrometry as well as some deficiencies of existing computer programs for the quantitative evaluation of spectra are discussed and some practical solutions are proposed. (author)

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 ...

An intercomparison of Monte Carlo codes used for in-situ gamma-ray spectrometry

International Nuclear Information System (INIS)

Hurtado, S.; Villa, M.

2010-01-01

In-situ gamma-ray spectrometry is widely used for monitoring of natural as well as man-made radionuclides and corresponding gamma fields in the environment or working places. It finds effective application in the operational and accidental monitoring of nuclear facilities and their vicinity, waste depositories, radioactive contamination measurements and environmental mapping or geological prospecting. In order to determine accurate radionuclide concentrations in these research fields, Monte Carlo codes have recently been used to obtain the efficiency calibration of in-situ gamma-ray detectors. This work presents an inter-comparison between two Monte Carlo codes applied to in-situ gamma-ray spectrometry. On the commercial market, Canberra has its LABSOCS/ISOCS software which is relatively inexpensive. The ISOCS mathematical efficiency calibration software uses a combination of Monte Carlo calculations and discrete ordinate attenuation computations. Efficiencies can be generated in a few minutes in the field and can be modified easily if needed. However, it has been reported in the literature that ISOCS computation method is accurate on average only within 5%, and additionally in order to use LABSOCS/ISOCS it is necessary a previous characterization of the detector by Canberra, which is an expensive process. On the other hand, the multipurpose and open source GEANT4 takes significant computer time and presents a non-friendly but powerful toolkit, independent of the manufacturer of the detector. Different experimental measurements of calibrated sources were performed with a Canberra portable HPGe detector and compared to the results obtained using both Monte Carlo codes. Furthermore, a variety of efficiency calibrations for different radioactive source distributions were calculated and tested, like plane shapes or containers filled with different materials such as soil, water, etc. LabSOCS simulated efficiencies for medium and high energies were given within an

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

Further development of IDGS: Isotope dilution gamma-ray spectrometry

International Nuclear Information System (INIS)

Li, T.K.; Parker, J.L.; Kuno, Y.; Sato, S.; Kamata, M.; Akiyama, T.

1991-01-01

The isotope dilution gamma-ray spectrometry (IDGS) technique for determining the plutonium concentration and isotopic composition of highly radioactive spent-fuel dissolver solutions has been further developed. Both the sample preparation and the analysis have been improved. The plutonium isotopic analysis is based on high-resolution, low-energy gamma-ray spectrometry. The plutonium concentration in the dissolver solutions then is calculated from the measured isotopic differences among the spike, the dissolver solution, and the spiked dissolver solution. Plutonium concentrations and isotopic compositions of dissolver solutions analyzed from this study agree well with those obtained by traditional isotope dilution mass spectrometry (IDMS) and are consistent with the first IDGS experimental result. With the current detector efficiency, sample size, and a 100-min count time, the estimated precision is ∼0.5% for 239 Pu and 240 Pu isotopic analyses and ∼1% for the plutonium concentration analysis. 5 refs., 2 figs., 7 tabs

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)

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

DEFF Research Database (Denmark)

Christensen, Leif Højslet; Heydorn, Kaj

1985-01-01

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

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)

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

Is scanning electron microscopy/energy dispersive X-ray spectrometry (SEM/EDS) quantitative?

Science.gov (United States)

Newbury, Dale E; Ritchie, Nicholas W M

2013-01-01

Scanning electron microscopy/energy dispersive X-ray spectrometry (SEM/EDS) is a widely applied elemental microanalysis method capable of identifying and quantifying all elements in the periodic table except H, He, and Li. By following the "k-ratio" (unknown/standard) measurement protocol development for electron-excited wavelength dispersive spectrometry (WDS), SEM/EDS can achieve accuracy and precision equivalent to WDS and at substantially lower electron dose, even when severe X-ray peak overlaps occur, provided sufficient counts are recorded. Achieving this level of performance is now much more practical with the advent of the high-throughput silicon drift detector energy dispersive X-ray spectrometer (SDD-EDS). However, three measurement issues continue to diminish the impact of SEM/EDS: (1) In the qualitative analysis (i.e., element identification) that must precede quantitative analysis, at least some current and many legacy software systems are vulnerable to occasional misidentification of major constituent peaks, with the frequency of misidentifications rising significantly for minor and trace constituents. (2) The use of standardless analysis, which is subject to much broader systematic errors, leads to quantitative results that, while useful, do not have sufficient accuracy to solve critical problems, e.g. determining the formula of a compound. (3) EDS spectrometers have such a large volume of acceptance that apparently credible spectra can be obtained from specimens with complex topography that introduce uncontrolled geometric factors that modify X-ray generation and propagation, resulting in very large systematic errors, often a factor of ten or more. © Wiley Periodicals, Inc.

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)

New portability for in situ gamma-ray spectrometry from commercially available equipment

International Nuclear Information System (INIS)

Stanford, N.; Laurenzo, E.L.; McCurdy, D.E.

1984-01-01

In situ gamma-ray spectrometry has been employed by the staff of the Yankee Atomic Environmental Laboratory on a routine basis for more than five years. The original in situ gamma-ray spectrometry methodology was adopted from the techniques developed at the DOE Environmental Measurements Laboratory (Beck, DeCampo, and Gogolak 1972). The system consisted of a 110 cm 3 Ge(Li) detector in the vertical configuration in conjunction with typical laboratory nuclear instrumentation, as well as a medium-sized desktop computer, printer and disk drive. The equipment was transported in a small van having a shock-mounted cabinet and gasoline generator as an electrical power source. Recent availability of miniaturized spectrometry systems and powerful portable computers has enabled the upgrading of the 1977 vintage equipment to a system which is truly portable, light weight, compact and more reliable. The system to be described utilizes a portable intrinsic germanium detector, a small, 4096 channel pulse height analyzer (MCA) with anscillary components and a 24K, Hewlett Packard HP-75 computer with a small tape drive. When the equipment is used in the field, the system has enough capability to acquire and store a full 4096 channel gamma-ray spectrum and calculate the soil concentrations (pCi/g) and/or external radiation exposure rates for the commonly found naturally occurring, long-lived atmospheric nuclear weapons testing and nuclear power plant radionuclides. Subsequent data transfer to a larger desktop computer via available interfacing at the laboratory enables a full peak search and a more extensive evaluation of the data in order to calculate the soil concentrations and/or external radiation exposure rates for a selected 25 radionuclides. Experiences from the first season of operation are discussed

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, ...

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

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

Continuous gamma-ray spectrometry in the fast flux test facility (FFTF)

International Nuclear Information System (INIS)

Gold, R.; Kaiser, B.J.; Moore, F.S. Jr.; Bunch, W.L.; McElroy, W.N.; Sheen, E.M.

1980-03-01

In-core Compton-recoil γ-ray spectrometry was carried out in FFTF at very low power in the In-Reactor Thimble (IRT). The lower-energy electron spectrum at the FFTF-IRT midplane and the unfolded γ-ray spectrum are shown. 2 figures

Conformational analysis of g protein-coupled receptor signaling by hydrogen/deuterium exchange mass spectrometry.

Science.gov (United States)

Li, Sheng; Lee, Su Youn; Chung, Ka Young

2015-01-01

Conformational change and protein-protein interactions are two major mechanisms of membrane protein signal transduction, including G protein-coupled receptors (GPCRs). Upon agonist binding, GPCRs change conformation, resulting in interaction with downstream signaling molecules such as G proteins. To understand the precise signaling mechanism, studies have investigated the structural mechanism of GPCR signaling using X-ray crystallography, nuclear magnetic resonance (NMR), or electron paramagnetic resonance. In addition to these techniques, hydrogen/deuterium exchange mass spectrometry (HDX-MS) has recently been used in GPCR studies. HDX-MS measures the rate at which peptide amide hydrogens exchange with deuterium in the solvent. Exposed or flexible regions have higher exchange rates and excluded or ordered regions have lower exchange rates. Therefore, HDX-MS is a useful tool for studying protein-protein interfaces and conformational changes after protein activation or protein-protein interactions. Although HDX-MS does not give high-resolution structures, it analyzes protein conformations that are difficult to study with X-ray crystallography or NMR. Furthermore, conformational information from HDX-MS can help in the crystallization of X-ray crystallography by suggesting highly flexible regions. Interactions between GPCRs and downstream signaling molecules are not easily analyzed by X-ray crystallography or NMR because of the large size of the GPCR-signaling molecule complexes, hydrophobicity, and flexibility of GPCRs. HDX-MS could be useful for analyzing the conformational mechanism of GPCR signaling. In this chapter, we discuss details of HDX-MS for analyzing GPCRs using the β2AR-G protein complex as a model system. © 2015 Elsevier Inc. All rights reserved.

Decreasing of the detection limit for gamma-ray Spectrometry with the influence of sample treatment

International Nuclear Information System (INIS)

Karami, M.; Sadighzadeh, A.; Asgharizadeh, F.; Sardari, D.; Tavassoli, A.; Arbabi, A.; Hochaghani, O.

2009-01-01

Full text: In this study the ash method has been applied for environmental sample treatment in order to decrease of the detection limit in gamma-ray spectrometry for low level radioactivity measurements. Detection limit in gamma ray spectrometry is the smallest expectation value of the net counting rate that can be detected on given probabilities. The environmental test samples have been changed into ash using a suitable oven. The heating were made under controlled temperature to avoid the escape of some radionuclides such as radiocaesium. The ash samples were measured by high resolution gamma-ray spectrometry system. (author)

Fast-ion energy resolution by one-step reaction gamma-ray spectrometry

DEFF Research Database (Denmark)

Salewski, Mirko; Nocente, M.; Gorini, G.

2016-01-01

The spectral broadening of γ-rays from fusion plasmas can be measured in high-resolution gamma-ray spectrometry (GRS). We derive weight functions that determine the observable velocity space and quantify the velocity-space sensitivity of one-step reaction high-resolution GRS measurements in magne...

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

The determination of molybdenum and tungsten in resin by x-ray-fluorescence spectrometry

International Nuclear Information System (INIS)

Eddy, B.T.

1985-01-01

This report describes a method using X-ray-fluorescence spectrometry for the determination of molybdenum and tungsten in ion-exchange resins. The dried resin is milled with sand, binder, and an internal-standard mixture before being briquetted. Niobium and zinc are used as the internal standards for molybdenum and tungsten respectively. Intensity measurements are made with the gold anode tube. Corrections are made for the interference of the Mo Kα analytical line on the background intensities used for the Mo Kα and Nb Kα lines. The precision of the analysis for molybdenum ranges from a relative standard deviation 0,02 at 5 mg/g to 0.045 at 55μg/g; for tungsten, the relative standard deviation ranges from 0,04 at 5 mg/g to 0,055 at 55μg/g. The limits of determination in the original resin sample were found to be 40μg/g for molybdenum and 80μg/g for tungsten. The laboratory method is given in an appendix

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

Standard guide for high-resolution gamma-ray spectrometry of soil samples

CERN Document Server

American Society for Testing and Materials. Philadelphia

2004-01-01

1.1 This guide covers the identification and quantitative determination of gamma-ray emitting radionuclides in soil samples by means of gamma-ray spectrometry. It is applicable to nuclides emitting gamma rays with an approximate energy range of 20 to 2000 keV. For typical gamma-ray spectrometry systems and sample types, activity levels of about 5 Bq (135 pCi) are measured easily for most nuclides, and activity levels as low as 0.1 Bq (2.7 pCi) can be measured for many nuclides. It is not applicable to radionuclides that emit no gamma rays such as the pure beta-emitting radionuclides hydrogen-3, carbon-14, strontium-90, and becquerel quantities of most transuranics. This guide does not address the in situ measurement techniques, where soil is analyzed in place without sampling. Guidance for in situ techniques can be found in Ref (1) and (2). This guide also does not discuss methods for determining lower limits of detection. Such discussions can be found in Refs (3), (4), (5), and (6). 1.2 This guide can be us...

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)

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

Science.gov (United States)

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

1990-01-01

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

Aircraft gamma-ray spectrometry in snow-water equivalent measurement

International Nuclear Information System (INIS)

Kuittinen, R.; Vironmaeki, J.

1979-01-01

During the winter periods 1976-1977 and 1977-1978 the Hydrological Office at the National Board of Waters and the Geological Survey of Finland carried out a joint study to evaluate usefuluess of gamma-ray spectrometry in snow-water equivalent measurement. A multichannel gamma-ray spectrometer was fitted in a DC-3 aircraft. Fourteen snow courses were operated using both the gravimetric method and the gamma-ray method. The snow courses were located in southern Finland in forest, swamp and agricultural land. The results shows that the gamma ray method can be considered suitable for use in Finnish conditions and the accuracy of the gamma-ray method is almost of the same magnitude as the accuracy of the gravimetric method. (Auth.)

Aircraft gamma-ray spectrometry in snow-water equivalent measurement

Energy Technology Data Exchange (ETDEWEB)

Kuittinen, R [National Board of Waters (Finland); Vironmaeki, J [Geological Survey of Finland

1979-01-01

During the winter periods 1976-1977 and 1977-1978 the Hydrological Office at the National Board of Waters and the Geological Survey of Finland carried out a joint study to evaluate usefuluess of gamma-ray spectrometry in snow-water equivalent measurement. A multichannel gamma-ray spectrometer was fitted in a DC-3 aircraft. Fourteen snow courses were operated using both the gravimetric method and the gamma-ray method. The snow courses were located in southern Finland in forest, swamp and agricultural land. The results shows that the gamma ray method can be considered suitable for use in Finnish conditions and the accuracy of the gamma-ray method is almost of the same magnitude as the accuracy of the gravimetric method.

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.

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.

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

Formic acid hydrolysis/liquid chromatography isotope dilution mass spectrometry: An accurate method for large DNA quantification.

Science.gov (United States)

Shibayama, Sachie; Fujii, Shin-Ichiro; Inagaki, Kazumi; Yamazaki, Taichi; Takatsu, Akiko

2016-10-14

Liquid chromatography-isotope dilution mass spectrometry (LC-IDMS) with formic acid hydrolysis was established for the accurate quantification of λDNA. The over-decomposition of nucleobases in formic acid hydrolysis was restricted by optimizing the reaction temperature and the reaction time, and accurately corrected by using deoxynucleotides (dNMPs) and isotope-labeled dNMPs as the calibrator and the internal standard, respectively. The present method could quantify λDNA with an expanded uncertainty of 4.6% using 10fmol of λDNA. The analytical results obtained with the present method were validated by comparing with the results of phosphate-base quantification by inductively coupled plasma-mass spectrometry (ICP-MS). The results showed good agreement with each other. We conclude that the formic acid hydrolysis/LC-IDMS method can quantify λDNA accurately and is promising as the primary method for the certification of DNA as reference material. Copyright © 2016 Elsevier B.V. All rights reserved.

Efficiency curves of NIRR-1 gamma-ray spectrometry system at near ...

African Journals Online (AJOL)

The full-energy peak efficiency curves of the gamma-ray spectrometry for use with the Nigeria Research Reactor-1 (NIRR-1) have been determined by both theoretical and experimental at two source-detector positions for routine neutron activation analysis. Standard gamma ray sources were used to determine the efficiency ...

Feasibility study of plutonium isotopic analysis of resin beads by nondestructive gamma-ray spectroscopy

International Nuclear Information System (INIS)

Li, T.K.

1985-01-01

We have initiated a feasibility study on the use of nondestructive low-energy gamma-ray spectroscopy for plutonium isotopic analysis on resin beads. Seven resin bead samples were measured, with each sample containing an average of 9 μg of plutonium; the isotopic compositions of the samples varied over a wide range. The gamma-ray spectroscopy results, obtained from 4-h counting-time measurements, were compared with mass spectrometry results. The average ratios of gamma-ray spectroscopy to mass spectrometry were 1.014 +- 0.025 for 238 Pu/ 239 Pu, 0.996 +- 0.018 for 240 Pu/ 239 Pu, and 0.980 +- 0.038 for 241 Pu/ 239 Pu. The rapid, automated, and accurate nondestructive isotopic analysis of resin beads may be very useful to process technicians and International Atomic Energy Agency inspectors. 3 refs., 1 fig., 3 tabs

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)

A simple source preparation method for alpha-ray spectrometry of volcanic rock sample

International Nuclear Information System (INIS)

Takahashi, Masaomi; Kurihara, Yuichi; Sato, Jun

2006-01-01

A simple source preparation method was developed for the alpha-ray spectrometry to determine U and Th in volcanic rockes. Isolation of U and Th from volcanic rocks was made by use of UTEVA-Spec. resin, extraction chromatograph material. U and Th were extracted by TTA-benzene solution and organic phase was evaporated drop by drop on a hot stainless steel planchet to dryness. This method was found to be effective for the preparation of sources for alpha-ray spectrometry. (author)

Demonstration of a collimated in situ method for determining depth distributions using gamma-ray spectrometry

CERN Document Server

Benke, R R

2002-01-01

In situ gamma-ray spectrometry uses a portable detector to quantify radionuclides in materials. The main shortcoming of in situ gamma-ray spectrometry has been its inability to determine radionuclide depth distributions. Novel collimator designs were paired with a commercial in situ gamma-ray spectrometry system to overcome this limitation for large area sources. Positioned with their axes normal to the material surface, the cylindrically symmetric collimators limited the detection of un attenuated gamma-rays from a selected range of polar angles (measured off the detector axis). Although this approach does not alleviate the need for some knowledge of the gamma-ray attenuation characteristics of the materials being measured, the collimation method presented in this paper represents an absolute method that determines the depth distribution as a histogram, while other in situ methods require a priori knowledge of the depth distribution shape. Other advantages over previous in situ methods are that this method d...

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.

Application of neutron activation techniques and x-ray energy dispersion spectrometry, in analysis of metallic traces adsorbed by chelex-100 resin

International Nuclear Information System (INIS)

Fernandes, Jair C.; Amaral, Angela M.; Magalhaes, Jesus C.; Pereira, Jose S.J.; Silva, Juliana B. da; Auler, Lucia M.L.A.

2000-01-01

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)

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

Hydrogen atoms can be located accurately and precisely by x-ray crystallography.

Science.gov (United States)

Woińska, Magdalena; Grabowsky, Simon; Dominiak, Paulina M; Woźniak, Krzysztof; Jayatilaka, Dylan

2016-05-01

Precise and accurate structural information on hydrogen atoms is crucial to the study of energies of interactions important for crystal engineering, materials science, medicine, and pharmacy, and to the estimation of physical and chemical properties in solids. However, hydrogen atoms only scatter x-radiation weakly, so x-rays have not been used routinely to locate them accurately. Textbooks and teaching classes still emphasize that hydrogen atoms cannot be located with x-rays close to heavy elements; instead, neutron diffraction is needed. We show that, contrary to widespread expectation, hydrogen atoms can be located very accurately using x-ray diffraction, yielding bond lengths involving hydrogen atoms (A-H) that are in agreement with results from neutron diffraction mostly within a single standard deviation. The precision of the determination is also comparable between x-ray and neutron diffraction results. This has been achieved at resolutions as low as 0.8 Å using Hirshfeld atom refinement (HAR). We have applied HAR to 81 crystal structures of organic molecules and compared the A-H bond lengths with those from neutron measurements for A-H bonds sorted into bonds of the same class. We further show in a selection of inorganic compounds that hydrogen atoms can be located in bridging positions and close to heavy transition metals accurately and precisely. We anticipate that, in the future, conventional x-radiation sources at in-house diffractometers can be used routinely for locating hydrogen atoms in small molecules accurately instead of large-scale facilities such as spallation sources or nuclear reactors.

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.

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.

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

Determination of vanadium in titanate-based ferroelectrics by INAA with discriminating gamma-ray spectrometry

Czech Academy of Sciences Publication Activity Database

Kameník, Jan; Dragounová, K.; Kučera, Jan; Bryknar, Z.; Trepakov, Vladimír; Strunga, Vladimír

2017-01-01

Roč. 311, č. 2 (2017), s. 1333-1338 ISSN 0236-5731. [1st International Conference on Radioanalytical and Nuclear chemistry (RANC). Budapest, 10.04.2016-15.04.2016] R&D Projects: GA ČR(CZ) GBP108/12/G108; GA MŠk LM2015056 Institutional support: RVO:68378271 ; RVO:61389005 Keywords : Titanate-based ferroelectrics * Vanadium * INAA * discriminating gamma-ray spectrometry Subject RIV: CB - Analytical Chemistry, Separation; BM - Solid Matter Physics ; Magnetism (FZU-D) OBOR OECD: Analytical chemistry; Condensed matter physics (including formerly solid state physics, supercond.) (FZU-D) Impact factor: 1.282, year: 2016

The accurate assessment of small-angle X-ray scattering data.

Science.gov (United States)

Grant, Thomas D; Luft, Joseph R; Carter, Lester G; Matsui, Tsutomu; Weiss, Thomas M; Martel, Anne; Snell, Edward H

2015-01-01

Small-angle X-ray scattering (SAXS) has grown in popularity in recent times with the advent of bright synchrotron X-ray sources, powerful computational resources and algorithms enabling the calculation of increasingly complex models. However, the lack of standardized data-quality metrics presents difficulties for the growing user community in accurately assessing the quality of experimental SAXS data. Here, a series of metrics to quantitatively describe SAXS data in an objective manner using statistical evaluations are defined. These metrics are applied to identify the effects of radiation damage, concentration dependence and interparticle interactions on SAXS data from a set of 27 previously described targets for which high-resolution structures have been determined via X-ray crystallography or nuclear magnetic resonance (NMR) spectroscopy. The studies show that these metrics are sufficient to characterize SAXS data quality on a small sample set with statistical rigor and sensitivity similar to or better than manual analysis. The development of data-quality analysis strategies such as these initial efforts is needed to enable the accurate and unbiased assessment of SAXS data quality.

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....

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)

Fast procedures for coincidence-summing correction in γ-ray spectrometry

International Nuclear Information System (INIS)

De Felice, Pierino; Angelini, Paola; Fazio, Aldo; Biagini, Roberto

2000-01-01

Simplified and fast procedures for coincidence-summing correction in γ-ray spectrometry were investigated. These procedures are based on the usual theoretical expressions of the correction factors, but differ in the determination of the total efficiency curve based on the following approximations: (a) replacement, below the knee efficiency value, of the total efficiency by the full-energy peak efficiency; and (b) use of linear interpolations (in log-log plot) between only two experimental points above the knee efficiency value; or (c) assumption of a peak-to-total efficiency ratio independent on the counting geometry; or (d) assumption of a constant relation between the peak-to-total efficiency ratios and the photoelectric-to-total cross section ratios. The above approximations were separately assumed for determination of the coincidence-summing correction factors for nuclides with complex decay scheme ( 133 Ba, 134 Cs, 152 Eu) and for 60 Co and 88 Y measured on a 15% relative efficiency p-type coaxial HPGe detector, for three source-detector geometries: point source placed on top of and at 10 cm from the detector window, and 1 l Marinelli beaker filled with aqueous solution. The results were compared with those based on more accurate experimental determinations of the total efficiency curve from measurements of standard sources of eight different single-γ-ray emitters. The usefulness of each simplified procedure is evaluated with respect to its accuracy and to the reduction of the number of standard sources and measurement time

Experimental determination of nuclear reaction rates (n,γ) by the gamma-rays capture spectrometry technique

International Nuclear Information System (INIS)

Lucatero, M.A.

1976-01-01

The technique of the gamma-rays capture spectrometry was used in the experimental determination of nuclear reaction rates of the type (n,γ). This technique consists in the incidence of a thermal neutrons collimated beam upon a sample, detecting the capture spectrum of gamma rays emitted at a solid fixed angle. In the determination of the efficiency curve intrinsic to the detection electronic system the reactions 199 Hg(n,γ) 200 Hg, 56 Fe(n,γ) 57 Fe and 63 Cu(n,γ) 64 Cu were used with the energy of the gamma rays capture of 5.976, 7.635 and 7.915 Mev respectively, through the irradiation of standard samples of Hg(175.3g), Fe(110.4g) and Cu(108.5g) of cylindrical geometry the two former and parallelepiped the latter. The problem concerning the corrections due to the thermal neutrons flux depression, the gammas auto-attenuation, and the geometric factor due to the cylindrical and parallelepiped geometry are involved in the data process. The experimental determination of the reaction 35 Cl(n,γ) 36 Cl rate was made through the observation of the gamma caputre of 6.111 Mev when a sample of CaCl 2 of cylindrical geometry was irradiated. This rate can be favorably compared with the reaction rate determined theoretically. (author)

Carborne gamma-ray spectrometry. Calibration and applications

International Nuclear Information System (INIS)

Aage, H.K.; Korsbech, U.; Bargholz, K.; Hovgaard, J.

2006-01-01

Calibration of carborne gamma-ray spectrometry systems for 137 Cs is carried out with a source successively placed at 791 positions within an area of 34 mx62 m. A computer model supplements the measurements. Hereby a sensitivity map for a surface contamination is generated as well as line and area sensitivities. Another model converts surface sensitivity to sensitivity for a deep contamination. Use of the sensitivity map for a non-homogeneous distribution of 137 Cs is demonstrated. Applications of line sensitivities for special tasks are discussed

Assessment of measurement result uncertainty in determination of 210Pb with the focus on matrix composition effect in gamma-ray spectrometry

International Nuclear Information System (INIS)

Iurian, A.R.; Pitois, A.; Kis-Benedek, G.; Migliori, A.; Padilla-Alvarez, R.; Ceccatelli, A.

2016-01-01

Reference materials were used to assess measurement result uncertainty in determination of 210 Pb by gamma-ray spectrometry, liquid scintillation counting, or indirectly by alpha-particle spectrometry, using its daughter 210 Po in radioactive equilibrium. Combined standard uncertainties of 210 Pb massic activities obtained by liquid scintillation counting are in the range 2–12%, depending on matrices and massic activity values. They are in the range 1–3% for the measurement of its daughter 210 Po using alpha-particle spectrometry. Three approaches (direct computation of counting efficiency and efficiency transfer approaches based on the computation and, respectively, experimental determination of the efficiency transfer factors) were applied for the evaluation of 210 Pb using gamma-ray spectrometry. Combined standard uncertainties of gamma-ray spectrometry results were found in the range 2–17%. The effect of matrix composition on self-attenuation was investigated and a detailed assessment of uncertainty components was performed. - Highlights: • Confirmed 210 Pb certified values by LSC and alpha-particle spectrometry ( 210 Po). • Assessed 210 Po measurement result uncertainty by alpha-particle spectrometry. • Matrix composition effect on gamma-ray spectrometry measurement result uncertainty. • Assessment of 210 Pb measurement result uncertainty by gamma-ray spectrometry. • Comparison of techniques and approaches: ‘fit-for-purpose’ considerations.

Development of isotope dilution gamma-ray spectrometry for plutonium analysis

Energy Technology Data Exchange (ETDEWEB)

Li, T.K.; Parker, J.L. (Los Alamos National Lab., NM (United States)); Kuno, Y.; Sato, S.; Kurosawa, A.; Akiyama, T. (Power Reactor and Nuclear Fuel Development Corp., Tokai, Ibaraki (Japan))

1991-01-01

We are studying the feasibility of determining the plutonium concentration and isotopic distribution of highly radioactive, spent-fuel dissolver solutions by employing high-resolution gamma-ray spectrometry. The study involves gamma-ray plutonium isotopic analysis for both dissolver and spiked dissolver solution samples, after plutonium is eluted through an ion-exchange column and absorbed in a small resin bead bag. The spike is well characterized, dry plutonium containing {approximately}98% of {sup 239}Pu. By using measured isotopic information, the concentration of elemental plutonium in the dissolver solution can be determined. Both the plutonium concentration and the isotopic composition of the dissolver solution obtained from this study agree well with values obtained by traditional isotope dilution mass spectrometry (IDMS). Because it is rapid, easy to operate and maintain, and costs less, this new technique could be an alternative method to IDMS for input accountability and verification measurements in reprocessing plants. 7 refs., 4 figs., 4 tabs.

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

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

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....

Screening in veterinary drug analysis and sports doping control based on full-scan, accurate-mass spectrometry

NARCIS (Netherlands)

Peters, R.J.B.; Stolker, A.A.M.; Mol, J.G.J.; Lommen, A.; Lyris, E.; Angelis, Y.S.; Vonaparti, A.; Stamou, M.; Georgakopoulos, C.G.; Nielen, M.W.F.

2010-01-01

A common trend in food contaminants and sports doping control is towards a limited number of targeted, full-scan, accurate-mass spectrometry (MS) methods based on time-of-flight (TOF) or Fourier-transform orbital trap (Orbitrap) mass analyzers. Retrospective analysis of the full-scan datasets of

Research on 3-D terrain correction methods of airborne gamma-ray spectrometry survey

International Nuclear Information System (INIS)

Liu Yanyang; Liu Qingcheng; Zhang Zhiyong

2008-01-01

The general method of height correction is not effectual in complex terrain during the process of explaining airborne gamma-ray spectrometry data, and the 2-D terrain correction method researched in recent years is just available for correction of section measured. A new method of 3-D sector terrain correction is studied. The ground radiator is divided into many small sector radiators by the method, then the irradiation rate is calculated in certain survey distance, and the total value of all small radiate sources is regarded as the irradiation rate of the ground radiator at certain point of aero- survey, and the correction coefficients of every point are calculated which then applied to correct to airborne gamma-ray spectrometry data. The method can achieve the forward calculation, inversion calculation and terrain correction for airborne gamma-ray spectrometry survey in complex topography by dividing the ground radiator into many small sectors. Other factors are considered such as the un- saturated degree of measure scope, uneven-radiator content on ground, and so on. The results of for- ward model and an example analysis show that the 3-D terrain correction method is proper and effectual. (authors)

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

Optimization of a neural network model for signal-to-background prediction in gamma-ray spectrometry

International Nuclear Information System (INIS)

Dragovic, S.; Onjia, A. . E-mail address of corresponding author: sdragovic@inep.co.yu; Dragovic, S.)

2005-01-01

The artificial neural network (ANN) model was optimized for the prediction of signal-to-background (SBR) ratio as a function of the measurement time in gamma-ray spectrometry. The network parameters: learning rate (α), momentum (μ), number of epochs (E) and number of nodes in hidden layer (N) were optimized simultaneously employing variable-size simplex method. The most accurate model with the root mean square (RMS) error of 0.073 was obtained using ANN with online backpropagation randomized (OBPR) algorithm with α = 0.27, μ 0.36, E = 14800 and N = 9. Most of the predicted and experimental SBR values for the eight radionuclides ( 226 Ra, 214 Bi, 235 U, 40 K, 232 Th, 134 Cs, 137 Cs and 7 Be), studied in this work, reasonably agreed to within 15 %, which was satisfactory accuracy. (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)

Investigation by gamma-ray spectrometry and INAA of radioactivity impact on phosphate fertilizer plant environment

International Nuclear Information System (INIS)

Pantelica, A.; Companis, I.; Georgescu, I. I.; Pincovshi, E.

2006-01-01

The radioactive polluting effect of a phosphate fertilizer plant on the environment was investigated by gamma-ray spectrometry and neutron activation analysis (INAA). The hazards could arise from industrial plants using raw phosphate materials to prepare fertilizers for agricultural purposes due to the phosphate rock which, depending on the type and geographical zone of provenance may contain rather large amounts of uranium. The fertilizer plant under study is situated about 4 km from the town of Turnu Magurele, on the left bank of the Danube River in Romania. The main by-products of the factory are: nitro phosphate type fertilizers (NP, NPK), Ammonia, Nitric acid, Ammonium nitrate, Urea, Sulfuric acid, Phosphoric acid, Sodium fluorosilicate and Aluminum sulfate. Gamma-ray spectrometry was used to determine activity concentrations of naturally occurring radionuclides ( 2 26Ra, 2 35U, 2 38U, 2 32Th, and 4 0K), as well as 1 37Cs man-made radionuclide in surface soils collected from semicircular areas within radii of 0.5 and 15 km of the plant; in addition, different NPK type fertilizers and phosphate rocks were investigated. The samples (mass of about 100-g each) were kept tightly closed for one month to permit 2 26Ra to establish radioactive equilibrium with its decay products. This method makes it possible to assess U, Th, and K contents in samples by measuring 2 38U and 2 32Th (in equilibrium with their radioactive daughters) and 4 0K radioactivity, taken into account that 1 g of U, Th and K yield 1 2358 Bq 2 38U, 569 Bq 2 35U, 4057.2 Bq 2 32Th and 33.11 Bq 4 0K, respectively. The spectrometrical chain was based on a HPGe (EG and G Ortec) detector of 30 % relative efficiency and 2.1 keV resolution at 1332 keV of 6 0Co. INAA technique (neutron irradiation at TRIGA reactor of SCN Pitesti) was used to determine macro, micro and trace elements in samples collected from both technological shops of the factory (air dust and drinking tap water) and its surroundings

Pulser injection with subsequent removal for gamma-ray spectrometry

International Nuclear Information System (INIS)

Hartwell, J.K.; Goodwin, S.G.; Johnson, L.O.; Killian, E.W.

1990-01-01

This patent describes a module for use with a gamma-ray spectroscopy system. The system includes a gamma-ray detector for detecting gamma-ray events and producing a signal representing the gamma-ray events, a converter responsive to the detector and capable of converting the signal to a spectrum, a storage memory responsive to the converter and capable of storing the spectrum at address locations in memory, and a pulser capable of injecting pulses into the signal produced by the detector. The module comprises: means for generating a logic pulse for controlling the pulser, the controlling means adapted for coupling to the pulser; means for generating separation of events logic to isolate the components of a combined gamma-ray---pulse spectrum, the separation of events logic means adapted for coupling to the converter and the storage memory with the capability of storing pulses at address locations in the storage memory separate from the gamma-ray events; means for receiving an imitating signal from the converter to generate a plurality of operations by the module; means for tracking variations in a gamma-ray---pulse spectrum brought on by external parameter changes; and means for interfacing with commercially developed gamma-ray spectrometry equipment

Peak-by-peak correction of Ge(Li) gamma-ray spectra for photopeaks from background

Energy Technology Data Exchange (ETDEWEB)

Cutshall, N H; Larsen, I L [Oak Ridge National Lab., TN (USA)

1980-12-01

Background photopeaks can interfere with accurate measurement of low levels of radionuclides by gamma-ray spectrometry. A flowchart for peak-by-peak correction of sample spectra to produce accurate results is presented.

Use of on-ground gamma-ray spectrometry to measure plant-available potassium and other topsoil attributes

International Nuclear Information System (INIS)

Wong, M.T.F.; Harper, R.J.

1999-01-01

The incidence of potassium (K) deficiency is increasing in crops, pastures, and forestry in south-western Australia. Although soil K can be measured using soil sampling and analysis, γ-ray spectrometry offers a potentially cheaper and spatially more precise alternative. This could be particularly useful in precision agriculture, where inputs are applied according to need rather than by general prescription. In a study of topsoils near Jerramungup, Western Australia, strong relationships (r 2 = 0.9) were found between on-ground counts of γ-rays derived from 40 K (γ-K) and both total K and plant-available K. The success of γ-ray spectrometry in predicting available K relied on a strong relationship (r 2 0.9) between total K and available K which may not hold in all areas. Although the relationship between γ-K and available K held over the range of 36-1012 mg/kg, crop response to K fertilisers is only expected when the available K content is 2 = 0.9) were also found between γ-K and a range of other soil attributes, including clay, silt, and organic carbon content. These relationships depended on the locally strong relationship between total K and these soil attributes. Since such relationships do not hold everywhere, the utility of γ-ray spectrometry will likewise be limited. Site-specific calibrations are required if γ-ray spectrometry is to be used for soil property mapping. Copyright (1999) CSIRO Publishing

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

Peak-by-peak correction of Ge(Li) gamma-ray spectra for photopeaks from background

International Nuclear Information System (INIS)

Cutshall, N.H.; Larsen, I.L.

1980-01-01

Background photopeaks can interfere with accurate measurement of low levels of radionuclides by gamma-ray spectrometry. A flowchart for peak-by-peak correction of sample spectra to produce accurate results is presented. (orig.)

Identification and accurate quantification of structurally related peptide impurities in synthetic human C-peptide by liquid chromatography-high resolution mass spectrometry.

Science.gov (United States)

Li, Ming; Josephs, Ralf D; Daireaux, Adeline; Choteau, Tiphaine; Westwood, Steven; Wielgosz, Robert I; Li, Hongmei

2018-06-04

Peptides are an increasingly important group of biomarkers and pharmaceuticals. The accurate purity characterization of peptide calibrators is critical for the development of reference measurement systems for laboratory medicine and quality control of pharmaceuticals. The peptides used for these purposes are increasingly produced through peptide synthesis. Various approaches (for example mass balance, amino acid analysis, qNMR, and nitrogen determination) can be applied to accurately value assign the purity of peptide calibrators. However, all purity assessment approaches require a correction for structurally related peptide impurities in order to avoid biases. Liquid chromatography coupled to high resolution mass spectrometry (LC-hrMS) has become the key technique for the identification and accurate quantification of structurally related peptide impurities in intact peptide calibrator materials. In this study, LC-hrMS-based methods were developed and validated in-house for the identification and quantification of structurally related peptide impurities in a synthetic human C-peptide (hCP) material, which served as a study material for an international comparison looking at the competencies of laboratories to perform peptide purity mass fraction assignments. More than 65 impurities were identified, confirmed, and accurately quantified by using LC-hrMS. The total mass fraction of all structurally related peptide impurities in the hCP study material was estimated to be 83.3 mg/g with an associated expanded uncertainty of 3.0 mg/g (k = 2). The calibration hierarchy concept used for the quantification of individual impurities is described in detail. Graphical abstract ᅟ.

Computer programs for data reduction and interpretation in plutonium and uranium analysis by gamma ray spectrometry

International Nuclear Information System (INIS)

Singh, R.K.; Moorthy, A.D.; Babbar, R.K.; Udagatti, S.V.

1989-01-01

Non destructive gamma ray have been developed for analysis of isotopic abundances and concentrations of plutonium and uranium in the respective product solutions of a reprocessing plant. The method involves analysis of gamma rays emitted from the sample and uses a multichannel analyser system. Data reduction and interpretation of these techniques are tedious and time consuming. In order to make it possible to use them in routine analysis, computer programs have been developed in HP-BASIC language which can be used in HP-9845B desktop computer. A set of programs, for plutonium estimation by high resolution gamma ray spectrometry and for on-line measurement of uranium by gamma ray spectrometry are described in this report. (author) 4 refs., 3 tabs., 6 figs

Determination of copper, iron and zinc in spirituous beverages by total reflection X-ray fluorescence spectrometry

Science.gov (United States)

Capote, T.; Marcó, L. M.; Alvarado, J.; Greaves, E. D.

1999-10-01

The concentration of copper in traditional homemade alcoholic distillates produced in Venezuela (Cocuy de Penca) were determined by total reflection X-ray fluorescence (TXRF) using vanadium as internal standard. The results were compared to those obtained by flame atomic absorption spectrometry (FAAS). Three preparative methods of addition of vanadium were compared: classical internal standard addition, 'layer on layer' internal standard addition and in situ addition of internal standard. The TXRF procedures were accurate and the precision was comparable to that obtained by the FAAS technique. Copper levels were above the maximum allowed limits for similar beverages. Zinc and iron in commercial and homemade distilled beverages were also analyzed by TXRF with in situ addition of internal standard demonstrating the usefulness of this technique for trace metal determination in distillates.

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

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)

Comparison of laser fluorimetry, high resolution gamma-ray spectrometry and neutron activation analysis techniques for determination of uranium content in soil samples

International Nuclear Information System (INIS)

Ghods, A.; Asgharizadeh, F.; Salimi, B.; Abbasi, A.

2004-01-01

Much more concern is given nowadays for exposure of the world population to natural radiation especially to uranium since 57% of that exposure is due to radon-222, which is a member of uranium decay series. Most of the methods used for uranium determination is low concentration require either tedious separation and preconcentration or the accessibility to special instrumentation for detection of uranium at this low level. this study compares three techniques and methods for uranium analysis among different soil sample with variable uranium contents. Two of these techniques, neutron activation analysis and high resolution gamma-ray spectrometry , are non-destructive while the other, laser fluorimetry is done via chemical extraction of uranium. Analysis of standard materials is done also to control the quality and accuracy of the work. In spite of having quite variable ranges of detection limit, results obtained by high resolution gamma-ray spectrometry based on the assumption of having secular equilibrium between uranium and its daughters, which causes deviation whenever this condition was missed. For samples with reasonable uranium content, neutron activation analysis would be a rapid and reliable technique, while for low uranium content laser fluorimetry would be the most appropriate and accurate technique

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

Open-source implementation of an algorithm for photopeaks search and analysis in gamma-ray spectrometry with semiconductor detectors

International Nuclear Information System (INIS)

Maduar, Marcelo F.; Pecequilo, Brigitte R.S.

2009-01-01

Radioactivity quantification of gamma-ray emitter radionuclides in samples measured by HPGe gamma spectrometers relies on the analysis of the photopeaks present in the spectra, especially on the accurate determination of their net areas. This paper presents a methodology and an algorithm description for the peak search and analysis in order to obtain the relevant peaks parameters and their uncertainties. The procedure is performed on a three step approach: a preliminary search is done by using the second-difference method; experimental peaks widths are assessed in order to obtain a width vs. channel relationship and to define regions with single or overlapping peaks; a non-linear fit is applied to each region of the spectrum with candidate peaks. The final target function is in the form G(x) = B(x) + F(x), where B(x) is the baseline composed by a sum of a weighed left-side B L (x) and right-side B R (x) base-line quadratic functions and the photopeaks term F(x) is a sum of Gaussian functions. The computational implementation is released entirely in open-source license. The code was developed in C++ language and the interface was developed with Qt GUI software toolkit. GNU scientific library, GSL, was employed to perform linear and non-linear fitting procedures as needed. Spectra previously generated at our laboratories were analyzed with the presented methodology and with the commercial software package WinnerGamma. Results obtained are consistent with those obtained with the aforementioned package, suggesting that it could be safely used in general-purpose gamma-ray spectrometry. (author)

Determination of trace elements in Katana (Japanese sword) by neutron activation analysis with multidimensional γ-ray spectrometry

International Nuclear Information System (INIS)

Okada, Y.; Hirai, S.; Ohya, S.; Kimura, Atsushi; Hatsukawa, Yuichi; Toh, Yosuke; Koizumi, Mitsuo; Oshima, Masumi

2006-01-01

In this study, we tried to measure trace elements (As and Sb) in Katana (Japanese swords) by multidimensional γ-ray spectrometry method (GEMINI-II) and conventional counting method for neutron activation analysis (NAA). The determined values by GEMINI-II and conventional counting were in good agreement with. Using the multidimensional γ-ray spectrometry (GEMINI-II) to determine As and Sb was improved by 7 times and 10 times compared with the conventional counting method. (author)

Spiked environmental matrix for use as a reference material for gamma-ray spectrometry: Production and homogeneity test

International Nuclear Information System (INIS)

Sobiech-Matura, K.; Máté, B.; Altzitzoglou, T.

2016-01-01

The application of a spiking method for reference material production and its utilisation for a food matrix is presented. The raw rice powder was tested by means of γ-ray spectrometry and spiked with a "1"3"7Cs solution. The spiked material was mixed and tested for homogeneity. The future use of the rice powder reference material after the entire characterisation cycle will be for γ-ray spectrometry method validation. - Highlights: • Spiking blank substance with a traceable radioactive solution • Spiked reference material for γ-ray emitting radionuclides in food matrix • Results of the homogeneity tests are presented

Radiochemical separation of {sup 231}Pa from siliceous cake prior to its determination by gamma ray spectrometry

Energy Technology Data Exchange (ETDEWEB)

Dalvi, Aditi A. [Bhabha Atomic Research Centre, Mumbai (India). Analytical Chemistry Div.; Homi Bhabha National Institute, Mumbai (India); Verma, Rakesh

2017-07-01

A simple and fast radiochemical method for the separation of protactinium ({sup 231}Pa) from siliceous cake for its determination by gamma ray spectrometry is described. The method involves (a) a novel approach, the fusion of the siliceous cake with sodium peroxide, (b) the dissolution of the fused mass in nitric acid and (c) the co-precipitation of {sup 231}Pa with manganese dioxide formed in-situ by the addition of solid manganous sulfate and potassium permanganate to the solution. The fusion, effected in a single step, is simpler and highly effective in comparison to methods reported hitherto in literature. The radiochemical yield of {sup 231}Pa, determined using 311.9 keV gamma ray of {sup 233}Pa radiotracer is quantitative (∝90%). The decontamination factors calculated using gamma ray spectrometry and energy dispersive X-ray fluorescence measurements show that the separation from the interfering radionuclides is high whereas separation from major and minor elements is good. Separation by ion-exchange method in hydrochloric acid, hydrofluoric acid and oxalic acid media have comparatively much lower yields. The concentration of {sup 231}Pa in the siliceous cake measured using interference-free 283.6 keV gamma ray was found to be (6.4 ± 0.33) μg kg{sup -1}. The measured concentration of {sup 231}Pa was well above the limit of quantitation whereas the coefficient of variation was ∝5%. The improvement in the limit of detection was due to the reduction in spectral background. Systematic evaluation of various uncertainty parameters showed that the major contributors to the combined uncertainty were efficiency of the high purity germanium detector and the counting statistics. The present sample decomposition and separation methods are robust, simple to perform and can be effectively used for the determination and hence source prospecting of protactinium.

Proceedings of the International Symposium Advances in alpha, Beta- and Gamma-Ray spectrometry

International Nuclear Information System (INIS)

1997-01-01

The International Committee for Radionuclide Metrology (ICRM) is an association of radionuclide metrology laboratories whose membership is composed of delegates of these laboratories together with other scientists actively engaged in the study and applications of radioactivity. The scientific activities are carried out in the frame of six Working Groups. Two of them, the Alpha-Particle Spectrometry and the Gamma-and Beta-ray Spectrometry Working Groups held a common workshop in Pushkin, St. Petersburg, 18 to 20 September 1996, under the title Advances in Alpha-Beta-and Gamma-Ray Sepectrometry, at the kind invitation of the D.I. Mendeleyev Institute for Metrology. More than 30 people from 14 laboratories attended the meeting, and nineteen oral communications were presented, from which twelve were retained for publication an are included in these proceedings. (Author)

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)

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

Accurate determination of non-metallic impurities in high purity tetramethylammonium hydroxide using inductively coupled plasma tandem mass spectrometry

Science.gov (United States)

Fu, Liang; Xie, Hualin; Shi, Shuyun; Chen, Xiaoqing

2018-06-01

The content of non-metallic impurities in high-purity tetramethylammonium hydroxide (HPTMAH) aqueous solution has an important influence on the yield, electrical properties and reliability of the integrated circuit during the process of chip etching and cleaning. Therefore, an efficient analytical method to directly quantify the content of non-metallic impurities in HPTMAH aqueous solutions is necessary. The present study was aimed to develop a novel method that can accurately determine seven non-metallic impurities (B, Si, P, S, Cl, As, and Se) in an aqueous solution of HPTMAH by inductively coupled plasma tandem mass spectrometry (ICP-MS/MS). The samples were measured using a direct injection method. In the MS/MS mode, oxygen and hydrogen were used as reaction gases in the octopole reaction system (ORS) to eliminate mass spectral interferences during the analytical process. The detection limits of B, Si, P, S, Cl, As, and Se were 0.31, 0.48, 0.051, 0.27, 3.10, 0.008, and 0.005 μg L-1, respectively. The samples were analyzed by the developed method and the sector field inductively coupled plasma mass spectrometry (SF-ICP-MS) was used for contrastive analysis. The values of these seven elements measured using ICP-MS/MS were consistent with those measured by SF-ICP-MS. The proposed method can be utilized to analyze non-metallic impurities in HPTMAH aqueous solution. Table S2 Multiple potential interferences on the analytes. Table S3 Parameters of calibration curve and the detection limit (DL). Table S4 Results obtained for 25% concentration high-purity grade TMAH aqueous solution samples (μg L-1, mean ± standard deviation, n = 10).

Determination of plutonium isotopic ratios and total concentration by gamma ray spectrometry

International Nuclear Information System (INIS)

Despres, Michele.

1980-11-01

A non-destructive method of analysis is being investigated for the control in situ of plutonium isotopic composition and total concentration in different matrix without preliminary calibration. The plutonium isotopic composition is determined by gamma-ray spectrometry using germanium detector systems. The same apparatus is used for direct measuring of the total plutonium concentration in solutions or solids by a differential attenuation technique based on two transmitted gamma rays with energies on both sides of the k shell absorption edge of plutonium [fr

Gamma-ray spectrometry of granitic suites of the Paranaguá Terrane, Southern Brazil

Science.gov (United States)

Weihermann, Jessica Derkacz; Ferreira, Francisco José Fonseca; Cury, Leonardo Fadel; da Silveira, Claudinei Taborda

2016-09-01

The Paranaguá Terrane, located in the coastal portion of the states of Santa Catarina, Paraná and São Paulo in Southern Brazil is a crustal segment constituted mainly by an igneous complex, with a variety of granitic rocks inserted into the Serra do Mar ridge. The average altitude is approximately 1200 m above sea level, with peaks of up to 1800 m. Due to the difficulty of accessing the area, a shortage of outcrops and the thick weathering mantle, this terrane is understudied. This research aims to evaluate the gamma-ray spectrometry data of the granitic suites of the Paranaguá Terrane, in correspondence with the geological, petrographical, lithogeochemical, relief and mass movement information available in the literature. Aerogeophysical data were acquired along north-south lines spaced at 500 m, with a mean terrain clearance of 100 m. These data cover potassium (K, %), equivalent in thorium (eTh, ppm) and equivalent in uranium (eU, ppm). After performing a critical analysis of the data, basic (K, eU, eTh) and ternary (R-K/G-eTh/B-eU) maps were generated and then superimposed on the digital elevation model (DEM). The investigation of the radionuclide mobility across the relief and weathering mantle consisted of an analysis of the schematic profiles of elevation related with each radionuclide; a comparison of the K, eU and eTh maps with their 3D correspondents; and the study of mass movements registered in the region. A statistical comparison of lithogeochemical (K, U, Th) and geophysical (K, eU, eTh) data showed consistency in all the granitic suites studied (Morro Inglês, Rio do Poço and Canavieiras-Estrela). Through gamma-ray spectrometry, it was possible to establish relationships between scars (from mass movements) and the gamma-ray responses as well as the radionuclide mobility and the relief and to map the granitic bodies.

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)

Gamma-ray spectrometry laboratory and in situ: developments and environmental applications

International Nuclear Information System (INIS)

Gasser, Estelle

2014-01-01

Gamma-ray spectrometry enables determining all γ-ray emitters in a sample with a single measurement. Self-absorption of γ-rays in samples is manifest by a loss or a gain of pulses that results in a poor estimation of the counting efficiency. To characterize a new counting geometry improvements of the existing set-up were made with MCNPX simulations. With the new geometry we could specify absorbed and annual effective doses as well as dose conversion factors for the natural radioisotopes of several building materials and soil samples. Simulations show the influence of detection limits of γ-radiation on dose conversion factors and the need for updating these factors. γ-ray measurements of soil in situ require different counting efficiencies simulated by MCNPX for a semi-infinite source. Two in-situ soil analyses were made, one around a nuclear power and the other for a private company. (author)

Classification of soil samples according to their geographic origin using gamma-ray spectrometry and principal component analysis

International Nuclear Information System (INIS)

Dragovic, Snezana; Onjia, Antonije

2006-01-01

A principal component analysis (PCA) was used for classification of soil samples from different locations in Serbia and Montenegro. Based on activities of radionuclides ( 226 Ra, 238 U, 235 U, 4 K, 134 Cs, 137 Cs, 232 Th and 7 Be) detected by gamma-ray spectrometry, the classification of soils according to their geographical origin was performed. Application of PCA to our experimental data resulted in satisfactory classification rate (86.0% correctly classified samples). The obtained results indicate that gamma-ray spectrometry in conjunction with PCA is a viable tool for soil classification

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.

Spectral-ratio radon background correction method in airborne γ-ray spectrometry based on compton scattering deduction

International Nuclear Information System (INIS)

Gu Yi; Xiong Shengqing; Zhou Jianxin; Fan Zhengguo; Ge Liangquan

2014-01-01

γ-ray released by the radon daughter has severe impact on airborne γ-ray spectrometry. The spectral-ratio method is one of the best mathematical methods for radon background deduction in airborne γ-ray spectrometry. In this paper, an advanced spectral-ratio method was proposed which deducts Compton scattering ray by the fast Fourier transform rather than tripping ratios, the relationship between survey height and correction coefficient of the advanced spectral-ratio radon background correction method was studied, the advanced spectral-ratio radon background correction mathematic model was established, and the ground saturation model calibrating technology for correction coefficient was proposed. As for the advanced spectral-ratio radon background correction method, its applicability and correction efficiency are improved, and the application cost is saved. Furthermore, it can prevent the physical meaning lost and avoid the possible errors caused by matrix computation and mathematical fitting based on spectrum shape which is applied in traditional correction coefficient. (authors)

Natural Radioactivity in Geological Samples from Algeria by SSNTD and γ-Ray Spectrometry

International Nuclear Information System (INIS)

Belafrites, A.

2009-01-01

Results of Solid State Nuclear Track Detector (SSNTD) measurements of natural radioactivity using contact autoradiography for the determination of uranium and non-contact autoradiography for radon emanation are presented. The study is complemented by gamma -ray spectrometric results. The SSNTD method applied to geological samples has given uranium concentrations consistent with those found by gamma -ray spectrometry. The results for uranium concentration and radon emanation show excellent agreement with the few values available in other works

Estimation of natural potassium concentration in Romanian males by in vivo gamma-ray spectrometry measurements

International Nuclear Information System (INIS)

Mirela Angela Saizu

2012-01-01

At the Whole Body Monitoring Laboratory, from IFIN-HH, Bucharest, Romania, there were performed in vivo gamma-ray spectrometry measurements on 108 Romanian males in order to evaluate the mineral natural potassium content in human body, as total value and concentration. The measurements were performed with a shadow shield whole body counter, tilted chair geometry, based on a shielded NaI(Tl) scintillation detector of 12.5 cm (diameter) x 10 cm (height) crystal size. The results revealed a calculated value of the mean total body potassium (TBK) of 135.03 ± 2.94 g and a value of 1.9 ± 0.022 g of potassium/kg of body weight for the mean body potassium concentration, for the measured males. These values are similar with the values declared for the Reference Man, in ICRP23. Correlations between total body potassium, potassium concentration and age, weight and Body Build Index were investigated and peculiar conclusions were resulted. (author)

In-depth glycoproteomic characterization of γ-conglutin by high-resolution accurate mass spectrometry.

Directory of Open Access Journals (Sweden)

Silvia Schiarea

Full Text Available The molecular characterization of bioactive food components is necessary for understanding the mechanisms of their beneficial or detrimental effects on human health. This study focused on γ-conglutin, a well-known lupin seed N-glycoprotein with health-promoting properties and controversial allergenic potential. Given the importance of N-glycosylation for the functional and structural characteristics of proteins, we studied the purified protein by a mass spectrometry-based glycoproteomic approach able to identify the structure, micro-heterogeneity and attachment site of the bound N-glycan(s, and to provide extensive coverage of the protein sequence. The peptide/N-glycopeptide mixtures generated by enzymatic digestion (with or without N-deglycosylation were analyzed by high-resolution accurate mass liquid chromatography-multi-stage mass spectrometry. The four main micro-heterogeneous variants of the single N-glycan bound to γ-conglutin were identified as Man2(Xyl (Fuc GlcNAc2, Man3(Xyl (Fuc GlcNAc2, GlcNAcMan3(Xyl (Fuc GlcNAc2 and GlcNAc 2Man3(Xyl (Fuc GlcNAc2. These carry both core β1,2-xylose and core α1-3-fucose (well known Cross-Reactive Carbohydrate Determinants, but corresponding fucose-free variants were also identified as minor components. The N-glycan was proven to reside on Asn131, one of the two potential N-glycosylation sites. The extensive coverage of the γ-conglutin amino acid sequence suggested three alternative N-termini of the small subunit, that were later confirmed by direct-infusion Orbitrap mass spectrometry analysis of the intact subunit.

Correction for sample self-absorption in activity determination by gamma spectrometry

International Nuclear Information System (INIS)

Galloway, R.B.

1991-01-01

Gamma ray spectrometry is a convenient method of determining the activity of the radioactive components in environmental samples. Commonly samples vary in gamma absorption or differ in absorption from the calibration standards available, so that accurate correction for self-absorption in the sample is essential. A versatile correction procedure is described. (orig.)

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

CERN Document Server

American Society for Testing and Materials. Philadelphia

2004-01-01

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

Smoothing technology of gamma-ray spectrometry data based on matched filtering

International Nuclear Information System (INIS)

Gu Min; Ge Liangquan

2009-01-01

Traditional method of smoothness of gamma-ray spectrometry data gives rise to aberration of spectra curves easily. The article improve convolution sliding transformation using idea of matched filtering. Gauss adding the exponential function instead of Gauss function is used as converting function. The improved method not only suppresses statistical fluctuation mostly but also keeps feature of spectra curves. Instance verified superiority of this new method. (authors)

Mapping the spatial distribution and activity of {sup 226}Ra at legacy sites through Machine Learning interpretation of gamma-ray spectrometry data

Energy Technology Data Exchange (ETDEWEB)

Varley, Adam, E-mail: a.l.varley@stir.ac.uk [Department of Biological and Environmental Sciences, University of Stirling, Stirling FK9 4LA (United Kingdom); Tyler, Andrew [Department of Biological and Environmental Sciences, University of Stirling, Stirling FK9 4LA (United Kingdom); Smith, Leslie [Department of Computing Science and Mathematics, University of Stirling, Stirling FK9 4LA (United Kingdom); Dale, Paul [Scottish Environmental Protection Agency, Radioactive Substances, Strathallan House, Castle Business Park, Stirling FK9 4TZ (United Kingdom); Davies, Mike [Nuvia Limited, The Library, Eight Street, Harwell Oxford, Didcot, Oxfordshire OX11 0RL (United Kingdom)

2016-03-01

Radium ({sup 226}Ra) contamination derived from military, industrial, and pharmaceutical products can be found at a number of historical sites across the world posing a risk to human health. The analysis of spectral data derived using gamma-ray spectrometry can offer a powerful tool to rapidly estimate and map the activity, depth, and lateral distribution of {sup 226}Ra contamination covering an extensive area. Subsequently, reliable risk assessments can be developed for individual sites in a fraction of the timeframe compared to traditional labour-intensive sampling techniques: for example soil coring. However, local heterogeneity of the natural background, statistical counting uncertainty, and non-linear source response are confounding problems associated with gamma-ray spectral analysis. This is particularly challenging, when attempting to deal with enhanced concentrations of a naturally occurring radionuclide such as {sup 226}Ra. As a result, conventional surveys tend to attribute the highest activities to the largest total signal received by a detector (Gross counts): an assumption that tends to neglect higher activities at depth. To overcome these limitations, a methodology was developed making use of Monte Carlo simulations, Principal Component Analysis and Machine Learning based algorithms to derive depth and activity estimates for {sup 226}Ra contamination. The approach was applied on spectra taken using two gamma-ray detectors (Lanthanum Bromide and Sodium Iodide), with the aim of identifying an optimised combination of detector and spectral processing routine. It was confirmed that, through a combination of Neural Networks and Lanthanum Bromide, the most accurate depth and activity estimates could be found. The advantage of the method was demonstrated by mapping depth and activity estimates at a case study site in Scotland. There the method identified significantly higher activity (< 3 Bq g{sup −1}) occurring at depth (> 0.4 m), that conventional gross

A new approach for the high-precision determination of the elemental uranium concentration in uranium ore by gamma-ray spectrometry

International Nuclear Information System (INIS)

Nagel, W.; Quik, F.

1993-01-01

A new approach for the determination of elemental uranium in uranium bearing ore, using high resolution gamma-ray spectrometry, was applied. Using a variant of the enrichment meter technique an agreement of better than 1% has been obtained between gamma-ray measurement results and the certified value obtained by other analytical methods. For the calibration of the gamma-ray spectrometer uranium reference samples have been used which are made available jointly in Europe and the USA as Certified Reference Materials for Gamma-ray Spectrometry (EC NRM 171 and NBS SRM 969, respectively). The measured ore has been put in a special designed container which ensured in all directions seen from the radiation window a uniform degree of infinite thickness of about 95%. The measurement results can be taken as an example for the applicability of gamma-ray spectrometry when high accuracy is required and under conditions where homogeneous distributed elemental uranium is embedded in a larger amount of matrix material. (author). 8 refs., 10 figs., 2 tabs., 2 appendices

Spectroscopic confirmation of the optical identification of X-ray sources used to determine accurate positions for the anomalous X-ray pulsars 1E 2259+58.6 and 4U 0142+61

Science.gov (United States)

van den Berg, M.; Verbunt, F.

2001-03-01

Optical spectra show that two proposed counterparts for X-ray sources detected near 1E 2259+58.6 are late G stars, and a proposed counterpart for a source near 4U 0142+61 is a dMe star. The X-ray luminosities are as expected for such stars. We thus confirm the optical identification of the three X-ray objects, and thereby the correctness of the accurate positions for 1E 2259+58.6 and 4U 0142+61 based on them. Based on observations made with the William Herschel Telescope operated on the island of La Palma by the Isaac Newton Group in the Spanish Observatorio del Roque de los Muchachos of the Instituto de Astrofisica de Canarias.

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)

Energy dispersive x-ray spectrometry by microcalorimetry for the SEM

CERN Document Server

Newbury, D; Sae Woo Nam; Hilton, G; Irwin, K; Small, J; Martinis, J

2002-01-01

Analytical x-ray spectrometry for electron beam instruments has advanced significantly with the development of the microcalorimeter energy dispersive x-ray spectrometer (mu cal EDS). The mu cal EDS operates by measuring the temperature rise when a single photon is absorbed in a metal target. A cryoelectronic circuit with electrothermal feedback and a superconducting transition edge sensor serves as the thermometer. Spectral resolution approaching 4.5 eV for high energy photons (6000 eV) and 2 eV for low energy photons below 2000 eV has been demonstrated in energy dispersive operation across a photon energy range from 250 eV to 8 keV. Spectra of a variety of materials demonstrate the power of the mu cal EDS to solve practical problems while operating on a scanning electron microscope platform. (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

Airborne gamma-ray spectrometry data processing using 1.5D inversion.

Science.gov (United States)

Druker, Eugene

2017-10-01

Standard processing of Airborne Gamma-Ray Spectrometry data generally gives good results when the measurement conditions are almost constant within several footprint area sizes, with the possible exception of flight height variations in a small range. In practice, deviations, such as large or abrupt changes of flight height and/or rugged terrain are not so rare and lead to certain problems. This article proposes a different approach where the solutions of inverse problems are used for data processing. The approach is quite natural in the processing of field data measured along the flight lines: it explicitly takes into account 1.5D survey models and flight parameters - from topography to sources distribution on the surface. Also, it clearly demonstrates that the inverse problem of the Airborne Gamma-Ray Spectrometry does not have a unique solution. This feature can be used in accordance with the underlying geological problem since various formulations of inverse problems can lead to various geological solutions. The use of the approach is illustrated by several examples given for flight lines and survey areas. This approach can be particularly useful in situations where geological, geophysical and/or geographic survey conditions are far from the standard assumptions. Copyright © 2017 Elsevier Ltd. All rights reserved.

Fourier Transform Mass Spectrometry and Nuclear Magnetic Resonance Analysis for the Rapid and Accurate Characterization of Hexacosanoylceramide.

Science.gov (United States)

Ross, Charles W; Simonsick, William J; Bogusky, Michael J; Celikay, Recep W; Guare, James P; Newton, Randall C

2016-06-28

Ceramides are a central unit of all sphingolipids which have been identified as sites of biological recognition on cellular membranes mediating cell growth and differentiation. Several glycosphingolipids have been isolated, displaying immunomodulatory and anti-tumor activities. These molecules have generated considerable interest as potential vaccine adjuvants in humans. Accurate analyses of these and related sphingosine analogues are important for the characterization of structure, biological function, and metabolism. We report the complementary use of direct laser desorption ionization (DLDI), sheath flow electrospray ionization (ESI) Fourier transform ion cyclotron resonance mass spectrometry (FTICR MS) and high-field nuclear magnetic resonance (NMR) analysis for the rapid, accurate identification of hexacosanoylceramide and starting materials. DLDI does not require stringent sample preparation and yields representative ions. Sheath-flow ESI yields ions of the product and byproducts and was significantly better than monospray ESI due to improved compound solubility. Negative ion sheath flow ESI provided data of starting materials and products all in one acquisition as hexacosanoic acid does not ionize efficiently when ceramides are present. NMR provided characterization of these lipid molecules complementing the results obtained from MS analyses. NMR data was able to differentiate straight chain versus branched chain alkyl groups not easily obtained from mass spectrometry.

Fourier Transform Mass Spectrometry and Nuclear Magnetic Resonance Analysis for the Rapid and Accurate Characterization of Hexacosanoylceramide

Directory of Open Access Journals (Sweden)

Charles W. Ross

2016-06-01

Full Text Available Ceramides are a central unit of all sphingolipids which have been identified as sites of biological recognition on cellular membranes mediating cell growth and differentiation. Several glycosphingolipids have been isolated, displaying immunomodulatory and anti-tumor activities. These molecules have generated considerable interest as potential vaccine adjuvants in humans. Accurate analyses of these and related sphingosine analogues are important for the characterization of structure, biological function, and metabolism. We report the complementary use of direct laser desorption ionization (DLDI, sheath flow electrospray ionization (ESI Fourier transform ion cyclotron resonance mass spectrometry (FTICR MS and high-field nuclear magnetic resonance (NMR analysis for the rapid, accurate identification of hexacosanoylceramide and starting materials. DLDI does not require stringent sample preparation and yields representative ions. Sheath-flow ESI yields ions of the product and byproducts and was significantly better than monospray ESI due to improved compound solubility. Negative ion sheath flow ESI provided data of starting materials and products all in one acquisition as hexacosanoic acid does not ionize efficiently when ceramides are present. NMR provided characterization of these lipid molecules complementing the results obtained from MS analyses. NMR data was able to differentiate straight chain versus branched chain alkyl groups not easily obtained from mass spectrometry.

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...

Development of low-energy X-ray spectrometry at the Laboratoire National Henri Becquerel

International Nuclear Information System (INIS)

Lepy, M.C.; Plagnard, J.

2007-01-01

In the frame of the French Metrology Institute, the Laboratoire National Henri Becquerel performs accurate characterization of semiconductor detectors that are in use in a number of applications. Their efficiency calibration, energy resolution and the detailed shape of their response function are parameters of interest for accurate processing of low-energy X-ray spectra to be applied to elements identification and fundamental research studies. The tools specifically developed for low-energy detectors calibration and characterization are described, from the use of radioactivity standard to the development of a tunable monochromatic X-ray source. (Author)

Several experimental applications of gamma ray spectrometry on the analysis of uranium compounds

International Nuclear Information System (INIS)

Korob, Ricardo O.; Blasiyh Nuno, Guillermo A.

2002-01-01

Several experimental applications of gamma ray spectrometry on the analysis of uranium compounds and materials containing it are studied. Special attention is devoted to the correlation between experimental spectra and the decay chains of 235 U and 238 U contained in the analyzed samples. The following applications are discussed: enrichment determination without using calibration standards, determination of uranium concentration, intensities of the gamma rays emitted by the nuclides present in the decay chains of study and the activity of such nuclides. Because of its importance, detailed discussion about the former one is shown. In addition, preliminary results regarding the emission probabilities of the most important gamma rays of 234m Pa are also informed. (author)

Gamma-ray scanning of neutron activated geological sediments for studying elemental profile distributions

International Nuclear Information System (INIS)

Ellinger, M.; Janghorbani, M.; Starke, K.

1976-01-01

Gamma-ray scanning for application to elemental profile studies of geological samples was studied with a neutron activated Baltic Shield sediment. Profile distribution of seven elements were measured. The capabilities and limitations of gamma-ray scanning are discussed by comparing the results with profiles obtained after the mechanical subdivision of the sample and the activation of the appropriately sized separates. With respect to the merits and limitations of scanning gamma-ray spectrometry applied to activated complex matrices the following conclusions were drawn. Qualitatively, the scanning method yields the same information as the much more laborious method of mechanical sudbisubdivision. Quantitatively, it is significantly less accurate. The scanning method has the significant advantage of allowing preservation of the sample. This could be important for such speciments as lunar and archeological materials. The method reduces sample preparation time and the possibility of sample contamination. (T.G.)

Using MALDI-TOF mass spectrometry as a rapid and accurate diagnostic tool in infective endocarditis: a case report of a patient with mitral valve infective endocarditis caused by Abiotrophia defectiva

DEFF Research Database (Denmark)

Holler, Jon Gitz; Pedersen, Line; Calum, Henrik

2011-01-01

A case of infective endocarditis caused by Abiotrophia defectiva is presented. The use of MALDI-TOF mass spectrometry as a rapid and accurate diagnostic tool in infective endocarditis is discussed.......A case of infective endocarditis caused by Abiotrophia defectiva is presented. The use of MALDI-TOF mass spectrometry as a rapid and accurate diagnostic tool in infective endocarditis is discussed....

Accurate determination of 41Ca concentrations in spent resins from the nuclear industry by Accelerator Mass Spectrometry

International Nuclear Information System (INIS)

Nottoli, Emmanuelle; Bourlès, Didier; Bienvenu, Philippe; Labet, Alexandre; Arnold, Maurice; Bertaux, Maité

2013-01-01

The radiological characterisation of nuclear waste is essential for managing storage sites. Determining the concentration of Long‐Lived RadioNuclides (LLRN) is fundamental for their long-term management. This paper focuses on the measurement of low 41 Ca concentrations in ions exchange resins used for primary fluid purification in Pressurised Water Reactors (PWR). 41 Ca concentrations were successfully measured by Accelerator Mass Spectrometry (AMS) after the acid digestion of resin samples, followed by radioactive decontamination and isobaric suppression through successive hydroxide, carbonate, nitrate and final CaF 2 precipitations. Measured 41 Ca concentrations ranged from 0.02 to 0.03 ng/g, i.e. from 0.06 to 0.09 Bq/g. The 41 Ca/ 60 Co activity ratios obtained were remarkably reproducible and in good agreement with the current ratio used for resins management. - Highlights: • In the context of radioactive waste management, this study aimed at measuring 41 Ca in spent resins using Accelerator Mass Spectrometry. • A chemical treatment procedure was developed to quantitatively recover calcium in solution and selectively extract it. • Developed firstly on synthetic matrices, the chemical treatment procedure was then successfully applied to real resin samples. • Accelerator mass spectrometry allowed measuring concentrations of 41 Ca in spent resins as low as 0.02 ng/g of dry resin. • Final results are in agreement with current data used for spent resins management

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

Accurate CpG and non-CpG cytosine methylation analysis by high-throughput locus-specific pyrosequencing in plants.

Science.gov (United States)

How-Kit, Alexandre; Daunay, Antoine; Mazaleyrat, Nicolas; Busato, Florence; Daviaud, Christian; Teyssier, Emeline; Deleuze, Jean-François; Gallusci, Philippe; Tost, Jörg

2015-07-01

Pyrosequencing permits accurate quantification of DNA methylation of specific regions where the proportions of the C/T polymorphism induced by sodium bisulfite treatment of DNA reflects the DNA methylation level. The commercially available high-throughput locus-specific pyrosequencing instruments allow for the simultaneous analysis of 96 samples, but restrict the DNA methylation analysis to CpG dinucleotide sites, which can be limiting in many biological systems. In contrast to mammals where DNA methylation occurs nearly exclusively on CpG dinucleotides, plants genomes harbor DNA methylation also in other sequence contexts including CHG and CHH motives, which cannot be evaluated by these pyrosequencing instruments due to software limitations. Here, we present a complete pipeline for accurate CpG and non-CpG cytosine methylation analysis at single base-resolution using high-throughput locus-specific pyrosequencing. The devised approach includes the design and validation of PCR amplification on bisulfite-treated DNA and pyrosequencing assays as well as the quantification of the methylation level at every cytosine from the raw peak intensities of the Pyrograms by two newly developed Visual Basic Applications. Our method presents accurate and reproducible results as exemplified by the cytosine methylation analysis of the promoter regions of two Tomato genes (NOR and CNR) encoding transcription regulators of fruit ripening during different stages of fruit development. Our results confirmed a significant and temporally coordinated loss of DNA methylation on specific cytosines during the early stages of fruit development in both promoters as previously shown by WGBS. The manuscript describes thus the first high-throughput locus-specific DNA methylation analysis in plants using pyrosequencing.

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

Using airborne GAMMA-ray spectrometry (uranium, thorium, potassium) to quantify weathering and erosion processes

International Nuclear Information System (INIS)

Carrier, F.

2005-01-01

The airborne gamma-ray spectrometry survey carried out on the Armorican Massif provided soil contents in U, Th and K in ppm. Chemical and mechanical erosion processes within a homogeneous geological unit have been estimated using their variations and those of the 137 Cs. Our new approach, based on a multivariate analysis (hierarchic ascending classification), integrates the airborne gamma-ray spectrometry data, with their broad spatial distribution, together with precisely located station data (major elements, traces and isotopic geochemistry) resulting from a soil and river water erosion products survey. The total export of potassium was estimated in any point of an area catchment (50-m resolution) until 17+2 t/km 2 /a for a 50-m thick weathering profile. Erosion study by river sampling provide important biases, for the perennial river does not integrate the whole range of erosion products: the geochemical signature of the valleys is currently more represented than plateau areas. (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

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)

Developments in gamma-ray spectrometry: systems, software, and methods-II. 4. High-Performance Digital Gamma-Ray Spectrometry

International Nuclear Information System (INIS)

Michael Momayezi

2001-01-01

This paper reviews recent advances in the field of digital spectrometry made by researchers at X-Ray Instrumentation Associates. All XIA spectrometers are based on a core architecture, which employs digitizing the input signal without shaping and applying all basic data processing in real time to the digital data stream coming out of the wave form digitizer. The real-time digital data processing includes filtering, triggering, pileup rejection, and even pulse shape analysis. In this paper we will describe some of those methods that go beyond emulating a conventional analog system in a digital environment. Rather we will concentrate mainly on methods that have no real equivalent in the analog world. In conventional spectrometers pulse pileup recognition is hardwired and serves a single purpose, namely to reject signals that occur too close to each other to allow for a precise measurement of their amplitude. For a digital device, which can also record wave forms, that would be an unfortunate limitation. The study of very short-lived radioactive isotopes is a case in point. If such an isotope is implanted into a detector in which it then decays by charged particle emission, the signature for the sought-after isotope is that of an implant pulse followed by one or more decay pulses from the isotope and its daughters. If the decay products can be absorbed in the same detector channel, as is the case for proton and alpha emitters in a Si-strip detector, then the isotope decay will show up as a pulse train coming from that detector channel. The difficulty usually is to find the few isotopes of interest amongst a huge background of long-lived or stable isotopes. With programmable pileup recognition logic it is possible to trigger specifically on pulse trains, rather than single pulses, thereby picking out very selectively the isotopes of interest. Analyzing the pulse shape of the incoming preamplifier signal proves to be very useful in many applications. The most obvious

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)

Final results of the PIDIE intercomparison exercise for the plutonium isotopic determination by gamma-ray spectrometry

International Nuclear Information System (INIS)

Morel, J.; Chauvenet, B.; Etcheverry, M.

1991-01-01

Final results from the PIDIE intercomparison exercise organised by the ESARDA Working Group on techniques and standards for non-destructive analysis are presented. The aim of this exercise carried out in 1988 was to test the gamma-ray spectroscopy methods used to determine the plutonium isotopic ratios in a large range of isotopic composition, in order to analyse the parameters and the error sources influencing the results. Sets of seven sealed samples of different plutonium isotopic composition were sent to nine participating laboratories. The final results with uncertainty indicators are reported; they are compared with complementary mass-spectrometry determinations. No important bias has been observed from this exercise. Significant improvements in plutonium isotopic determination by gamma-ray spectrometry come from both more elaborate spectrum analysis methods and better equipment

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.

Analysis of spectra from portable handheld gamma-ray spectrometry for terrain comparative assessment

International Nuclear Information System (INIS)

Dias, Flávio; Lima, Marco; Sanjurjo-Sánchez, Jorge; Alves, Carlos

2016-01-01

Geological characteristics can have impacts on societal development by, e.g., geotechnical issues and radiological hazard levels. Due to urban sprawl, there is an increasing need for detailed geological assessment. In this work are analysed data from portable handheld gamma-ray spectra (K, eU and eTh) obtained in granitic and Silurian metaclastic outcrops as well as in an profile, roughly N–S, on soil covered terrains transecting a mapped contact between these rock types (the profile's northern extremity is at locations mapped as granite). Estimations from gamma-ray spectra were studied by univariate and multivariate analyses. K, eU and eTh values were higher on granite in relation to Silurian metaclastic rocks. The northern extremity of the profile showed clearly higher contents of eTh and this contrast was supported by univariate statistical tools (normality plot and Wilk–Shapiro test; boxplots). A ternary plot with the contribution of the elements to gamma-ray absorbed dose showed the separation of granite from Silurian metaclastic rocks with the former being nearer the eTh vertex. The points in the northern extremity of the profile are nearer the eTh vertex than the other points on the profile. These visual suggestions were supported by hierarchical cluster analysis, which was able to differentiate between granite and metaclastic outcrops and separate portions of the profile located on different terrains. Portable gamma-ray spectrometry showed, hence, the potential to distinguish granite and metaclastic terrains at a scale useful for engineering works. These results can also be useful for a first comparative zoning of radiological hazards (which are higher for granite). - Highlights: • Contents of K, eU and eTh were estimated by portable gamma-ray spectra. • Spectra were acquired on a profile across a soil covered granite/metaclastic contact. • Spectra were also collected on granite and Silurian metaclastic outcrops. • Obtained estimations were

Measurement of the G-value for 1. 5 keV X-rays

Energy Technology Data Exchange (ETDEWEB)

Freyer, J.P.; Schillaci, M.E.; Raju, M.R. (Los Alamos National Lab., NM (USA))

1989-12-01

Using a ferrous sulfate solution modified by the addition of benzoic acid, the authors measured relative G-values for Al{sub k} characteristic X-rays (1.5keV), {sup 238}Pu {alpha}-particles (3.7MeV), {sup 60}Co (1.17 MeV) and {sup 137}Cs (0.66 MeV){gamma}-rays. Relative ferrous-to-ferric conversions as a function of dose were similar for the two {gamma}-ray energies, yielding G-values of 1.62 and 1.59 {mu}mol J{sup -1} for the {sup 60}Co and {sup 137}Cs radiations. The {alpha}-particle G-value was 0.52 {mu}mol J{sup -1}, or 31% of that for {sup 60}Co {gamma}-rays. The Al{sub k} X-rays had a G-value of 0.92 {mu}mol J{sup -1} or 57% of that of the {sup 60}Co radiation. This G-value for 1.5 keV X-rays is within 20% of values predicted by current theories, and theoretical values are within the error range of the authors' measurements. (author).

Airborne gamma-ray spectrometry and computer data processing

International Nuclear Information System (INIS)

Raghuwanshi, S.S.; Bhishma Kumar; Tewari, S.G.

1993-01-01

The physical basis for the measurement of radioelemental concentrations of U, Th, and K on the surface of the earth by airborne gamma-ray spectrometry (AGRS) are described in this paper. The yield of an infinite radioactive plane source for a particular gamma energy helps to know the sampled volume in AGRS, the ground coverage, the ground resolution, the effective planning of the survey, flight line spacing, and sampling time. The infinite source-yield enables the determination of the attenuation coefficients in actual surveys and lays down the criteria for a standard test strip. Scattering of gamma-rays in matter is discussed in order to study its influence in the measurements from air. The theoretical gamma-ray spectrum from terrestrial U, Th, and K are discussed in contrast to its realistic picture which poses problems for their direct use for measurements. The criterion of FWHM (full width at half maximum) and inter-energy distance with their yields is described which finally helps to select the energy windows for (window and MCA) AGRS system. Factors which affect the measurements of radioelemental concentration in AGRS surveys include both correctable and non-correctable ones. Correctable factors are : (a) non-terrestrial sources of gamma-rays aircraft, cosmic, and airborne background (H) (B); (b) interference due to gamma-scattering inter channel effects (l); (c) height variations (H) due to navigation and topography; (d) temperature (T) of ambient air; and (e) pressure (P) of air at flying altitude. For removal of background effects, measurements over test strip and calibration pads are necessary for making the corrections in the order - BIH. These methods are described in the paper. The non-correctable factors include effects, due to terrain moisture, vegetation, and others. The possible ways to eliminate these effects are also briefly described. (author). 17 refs., 13 figs

High-z semiconductor nuclear radiation detectors for room-temperature gamma-ray spectrometry

International Nuclear Information System (INIS)

Bornand, Bernard; Friant, Alain.

1978-09-01

A bibliographical review (182 articles of periodicals, conferences, reports, thesis and french patents) is presented, as addendum of the report CEA-BIB-210 (1974) on high-Z semiconductor compounds used as materials for the gamma and X-ray detection and spectrometry. This publication reviews issues from 1974 to 1977. References and summaries (in french) are incorporated into 182 bibliograhical notices. Index for authors, corporate authors, documents and periodicals, and subjects is included [fr

INTERACTION OF ALBUMIN AND IMMUNOGLOBULIN G WITH SYNTHETIC HYDROXYAPATITE

Directory of Open Access Journals (Sweden)

E. Pylypchuk

2012-12-01

Full Text Available It was shown by X-ray phase analysis, IR spectra analysis and MALDI-ToF mass spectrometry methods that interaction of synthetic hydroxyapatite with a solution of immunoglobulin G leads to its partial dissolution due to leaching from the surface of calcium triphosphate which, in our opinion, forms complexes with immunoglobulin G.

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

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

Correcting the effects of the matrix using capture gamma-ray spectrometry: Application to measurement by Active Neutron Interrogation

International Nuclear Information System (INIS)

Baudry, G.

2003-11-01

In the field of the measurement of low masses of fissile material ( 235 U, 239 Pu, 241 Pu) in radioactive waste drums, the Active Neutron Interrogation is a non-destructive method achieving good results. It does however remain reliant upon uncertainties related to the matrix effects on interrogation and fission neutrons. The aim of this thesis is to develop a correction method able to take into account these matrix effects by quantifying the amount of absorbent materials (chlorine and hydrogen) in a 118- liter homogeneous matrix. The main idea is to use the gamma-ray spectrometry of gamma emitted by neutron captures to identify and quantify the composition of the matrix. An indicator from its chlorine content is then deduced in order to choose the calibration coefficient which best represents the real composition of the matrix. This document firstly presents the needs of control and characterization of radioactive objects, and the means used in the field of nuclear measurement. Emphases is put in particular on the Active Neutron Interrogation method. The matrices of interest are those made of light technological waste (density ≤ 0,4 g/cm 3 ) containing hydrogenated and chlorinated materials. The advantages of gamma-rays emitted by neutron captures for the determination of a chlorine content indicator of the matrices and the principles of the correction method are then explained. Measurements have been firstly realized with an existing Neutron Interrogation device (PROMETHEE 6). Such measurements have proven its inadequacy: no signal from the matrix hydrogen was detected, due to an intense signal from the polyethylene contained in some cell elements. Moreover, the matrix chlorine content appeared difficult to be measured. A new and specific device, named REGAIN and dedicated to active gamma-rays spectrometry, was defined with the Monte-Carlo N-Particle (MCNP) code. The experiments conducted with this new device made it possible to detect the hydrogen from the

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)

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.

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 radon concentration in soil gas by gamma-ray spectrometry of olive oil

International Nuclear Information System (INIS)

Al-Azmi, Darwish; Karunakara, N.

2007-01-01

Measurements of radon concentration in soil gas have been carried out using a bubbling system in which the soil gas is drawn through an active pumping to bubble a liquid absorber (olive oil) for the deposition of the soil gas in it. After the bubbling process, the absorber is then taken for gamma-ray measurements. Gamma-ray photopeaks from the 214 Pb and the 214 Bi radon progeny are considered for the detection of the 222 Rn gas to study the concentration levels for radon soil gas. Results for some field measurements were obtained and compared with results obtained using AlphaGuard radon gas monitor. The technique provides a possible approach for the measurements of radon soil gas with gamma-ray spectrometry

A simple method for the deconvolution of 134 Cs/137 Cs peaks in gamma-ray scintillation spectrometry

International Nuclear Information System (INIS)

Darko, E.O.; Osae, E.K.; Schandorf, C.

1998-01-01

A simple method for the deconvolution of 134 Cs / 137 Cs peaks in a given mixture of 134 Cs and 137 Cs using Nal(TI) gamma-ray scintillation spectrometry is described. In this method the 795 keV energy of 134 Cs is used as a reference peak to calculate the activity of the 137 Cs directly from the measured peaks. Certified reference materials were measured using the method and compared with a high resolution gamma-ray spectrometry measurements. The results showed good agreement with the certified values. The method is very simple and does not need any complicated mathematics and computer programme to de- convolute the overlapping 604.7 keV and 661.6 keV peaks of 134 Cs and 137 Cs respectively. (author). 14 refs.; 1 tab., 2 figs

Accurate quantification of 5 German cockroach (GCr) allergens in complex extracts using multiple reaction monitoring mass spectrometry (MRM MS).

Science.gov (United States)

Mindaye, S T; Spiric, J; David, N A; Rabin, R L; Slater, J E

2017-12-01

German cockroach (GCr) allergen extracts are complex and heterogeneous products, and methods to better assess their potency and composition are needed for adequate studies of their safety and efficacy. The objective of this study was to develop an assay based on liquid chromatography and multiple reaction monitoring mass spectrometry (LC-MRM MS) for rapid, accurate, and reproducible quantification of 5 allergens (Bla g 1, Bla g 2, Bla g 3, Bla g 4, and Bla g 5) in crude GCr allergen extracts. We first established a comprehensive peptide library of allergens from various commercial extracts as well as recombinant allergens. Peptide mapping was performed using high-resolution MS, and the peptide library was then used to identify prototypic and quantotypic peptides to proceed with MRM method development. Assay development included a systematic optimization of digestion conditions (buffer, digestion time, and trypsin concentration), chromatographic separation, and MS parameters. Robustness and suitability were assessed following ICH (Q2 [R1]) guidelines. The method is precise (RSD  0.99, 0.01-1384 fmol/μL), and sensitive (LLOD and LLOQ MS, we quantified allergens from various commercial GCr extracts and showed considerable variability that may impact clinical efficacy. Our data demonstrate that the LC-MRM MS method is valuable for absolute quantification of allergens in GCr extracts and likely has broader applicability to other complex allergen extracts. Definitive quantification provides a new standard for labelling of allergen extracts, which will inform patient care, enable personalized therapy, and enhance the efficacy of immunotherapy for environmental and food allergies. © 2017 The Authors. Clinical & Experimental Allergy published by John Wiley & Sons Ltd. This article has been contributed to by US Government employees and their work is in the public domain in the USA.

KRAS G12C Drug Development: Discrimination between Switch II Pocket Configurations Using Hydrogen/Deuterium-Exchange Mass Spectrometry

Energy Technology Data Exchange (ETDEWEB)

Lu, Jia; Harrison, Rane A.; Li, Lianbo; Zeng, Mei; Gondi, Sudershan; Scott, David; Gray, Nathanael S.; Engen, John R.; Westover, Kenneth D. (NEU); (DFCI); (UTSMC); (Harvard-Med)

2017-09-01

KRAS G12C, the most common RAS mutation found in non-small-cell lung cancer, has been the subject of multiple recent covalent small-molecule inhibitor campaigns including efforts directed at the guanine nucleotide pocket and separate work focused on an inducible pocket adjacent to the switch motifs. Multiple conformations of switch II have been observed, suggesting that switch II pocket (SIIP) binders may be capable of engaging a range of KRAS conformations. Here we report the use of hydrogen/deuterium-exchange mass spectrometry (HDX MS) to discriminate between conformations of switch II induced by two chemical classes of SIIP binders. We investigated the structural basis for differences in HDX MS using X-ray crystallography and discovered a new SIIP configuration in response to binding of a quinazoline chemotype. These results have implications for structure-guided drug design targeting the RAS SIIP.

Natural gamma-ray spectrometry as a tool for radiation dose and radon hazard modelling

International Nuclear Information System (INIS)

Verdoya, M.; Chiozzi, P.; De Felice, P.; Pasquale, V.; Bochiolo, M.; Genovesi, I.

2009-01-01

We reviewed the calibration procedures of gamma-ray spectrometry with particular emphasis to factors that affect accuracy, detection limits and background radiation in field measurements for dosimetric and radon potential mapping. Gamma-ray spectra were acquired in western Liguria (Italy). The energy windows investigated are centred on the photopeaks of 214 Bi (1.76 MeV), 208 Tl (2.62 MeV) and 40 K (1.46 MeV). The inferred absorbed dose rate and the radon flux are estimated to be lower than 60 nGy h -1 and 22 Bq m -2 h -1 , respectively.

New technique for determination of long-lived radioisotopes, Iodine-129, using multiparameter coincidence spectrometry

International Nuclear Information System (INIS)

Hatsukawa, Yuichi; Oshima, Masumi; Toh, Yosuke; Shinohara, Nobuo; Kushita, Kosuke; Ueno, Takashi

2003-01-01

Multiparameter coincidence γ-ray spectrometry based on g-g coincidence is widely used in the field of nuclear structure studies, and has produced many successful results. In this study, feasibility of the method for neutron activation analysis of long lived iodine isotope, 129 I, was investigated. (author)

Specialized software utilities for gamma ray spectrometry. Final report of a co-ordinated research project 1996-2000

International Nuclear Information System (INIS)

2002-03-01

A Co-ordinated Research Project (CRP) on Software Utilities for Gamma Ray Spectrometry was initiated by the International Atomic Energy Agency in 1996 for a three year period. In the CRP several basic applications of nuclear data handling were assayed which also dealt with the development of PC computer codes for various spectrometric purposes. The CRP produced several software packages: for the analysis of low level NaI spectra; user controlled analysis of gamma ray spectra from HPGe detectors; a set of routines for the definition of the detector resolution function and for the unfolding of experimental annihilation spectra; a program for the generation of gamma ray libraries for specific applications; a program to calculate true coincidence corrections; a program to calculate full-energy peak efficiency calibration curve for homogenous cylindrical sample geometries including self-attenuation correction; and a program for the library driven analysis of gamma ray spectra and for the quantification of radionuclide content in samples. In addition, the CRP addressed problems of the analysis of naturally occurring radioactive soil material gamma ray spectra, questions of quality assurance and quality control in gamma ray spectrometry, and verification of the expert system SHAMAN for the analysis of air filter spectra obtained within the framework of the Comprehensive Nuclear Test Ban Treaty. This TECDOC contains 10 presentations delivered at the meeting with the description of the software developed. Each of the papers has been indexed separately

Mass spectrometry of long-lived radionuclides

International Nuclear Information System (INIS)

Becker, Johanna Sabine.

2003-01-01

The capability of determining element concentrations at the trace and ultratrace level and isotope ratios is a main feature of inorganic mass spectrometry. The precise and accurate determination of isotope ratios of long-lived natural and artificial radionuclides is required, e.g. for their environmental monitoring and health control, for studying radionuclide migration, for age dating, for determining isotope ratios of radiogenic elements in the nuclear industry, for quality assurance and determination of the burn-up of fuel material in a nuclear power plant, for reprocessing plants, nuclear material accounting and radioactive waste control. Inorganic mass spectrometry, especially inductively coupled plasma mass spectrometry (ICP-MS) as the most important inorganic mass spectrometric technique today, possesses excellent sensitivity, precision and good accuracy for isotope ratio measurements and practically no restriction with respect to the ionization potential of the element investigated--therefore, thermal ionization mass spectrometry (TIMS), which has been used as the dominant analytical technique for precise isotope ratio measurements of long-lived radionuclides for many decades, is being replaced increasingly by ICP-MS. In the last few years instrumental progress in improving figures of merit for the determination of isotope ratio measurements of long-lived radionuclides in ICP-MS has been achieved by the application of a multiple ion collector device (MC-ICP-MS) and the introduction of the collision cell interface in order to dissociate disturbing argon-based molecular ions, to reduce the kinetic energy of ions and neutralize the disturbing noble gas ions (e.g. of 129 Xe + for the determination of 129 I). The review describes the state of the art and the progress of different inorganic mass spectrometric techniques such as ICP-MS, laser ablation ICP-MS vs. TIMS, glow discharge mass spectrometry, secondary ion mass spectrometry, resonance ionization mass

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)

A differential mobility spectrometry/mass spectrometry platform for the rapid detection and quantitation of DNA adduct dG-ABP.

Science.gov (United States)

Kafle, Amol; Klaene, Joshua; Hall, Adam B; Glick, James; Coy, Stephen L; Vouros, Paul

2013-07-15

There is continued interest in exploring new analytical technologies for the detection and quantitation of DNA adducts, biomarkers which provide direct evidence of exposure and genetic damage in cells. With the goal of reducing clean-up steps and improving sample throughput, a Differential Mobility Spectrometry/Mass Spectrometry (DMS/MS) platform has been introduced for adduct analysis. A DMS/MS platform has been utilized for the analysis of dG-ABP, the deoxyguanosine adduct of the bladder carcinogen 4-aminobiphenyl (4-ABP). After optimization of the DMS parameters, each sample was analyzed in just 30 s following a simple protein precipitation step of the digested DNA. A detection limit of one modification in 10^6 nucleosides has been achieved using only 2 µg of DNA. A brief comparison (quantitative and qualitative) with liquid chromatography/mass spectrometry is also presented highlighting the advantages of using the DMS/MS method as a high-throughput platform. The data presented demonstrate the successful application of a DMS/MS/MS platform for the rapid quantitation of DNA adducts using, as a model analyte, the deoxyguanosine adduct of the bladder carcinogen 4-aminobiphenyl. Copyright © 2013 John Wiley & Sons, Ltd.

Negative chemical ionization gas chromatography coupled to hybrid quadrupole time-of-flight mass spectrometry and automated accurate mass data processing for determination of pesticides in fruit and vegetables.

Science.gov (United States)

Besil, Natalia; Uclés, Samanta; Mezcúa, Milagros; Heinzen, Horacio; Fernández-Alba, Amadeo R

2015-08-01

Gas chromatography coupled to high resolution hybrid quadrupole time-of-flight mass spectrometry (GC-QTOF MS), operating in negative chemical ionization (NCI) mode and combining full scan with MSMS experiments using accurate mass analysis, has been explored for the automated determination of pesticide residues in fruit and vegetables. Seventy compounds were included in this approach where 50 % of them are not approved by the EU legislation. A global 76 % of the analytes could be identified at 1 μg kg(-1). Recovery studies were developed at three concentration levels (1, 5, and 10 μg kg(-1)). Seventy-seven percent of the detected pesticides at the lowest level yielded recoveries within the 70 %-120 % range, whereas 94 % could be quantified at 5 μg kg(-1), and the 100 % were determined at 10 μg kg(-1). Good repeatability, expressed as relative standard deviation (RSD home-made database was developed and applied to an automatic accurate mass data processing. Measured mass accuracies of the generated ions were mainly less than 5 ppm for at least one diagnostic ion. When only one ion was obtained in the single-stage NCI-MS, a representative product ion from MSMS experiments was used as identification criterion. A total of 30 real samples were analyzed and 67 % of the samples were positive for 12 different pesticides in the range 1.0-1321.3 μg kg(-1).

Improved microwave-assisted wet digestion procedures for accurate Se determination in fish and shellfish by flow injection-hydride generation-atomic absorption spectrometry

International Nuclear Information System (INIS)

Lavilla, I.; Gonzalez-Costas, J.M.; Bendicho, C.

2007-01-01

Accurate determination of Se in biological samples, especially fish and shellfish, by hydride generation techniques has generally proven troublesome owing to the presence of organoselenium that cannot readily converted into inorganic selenium under usual oxidising conditions. Further improvements in the oxidation procedures are needed so as to obtain accurate concentration values when this type of samples is analyzed. Microwave-assisted wet digestion (MAWD) procedures of seafood based on HNO 3 or the mixture HNO 3 /H 2 O 2 and further thermal reduction of the Se(VI) formed to Se(IV) were evaluated. These procedures were as follows: (I) without H 2 O 2 and without heating to dryness; (II) without H 2 O 2 and with heating to dryness; (III) with H 2 O 2 and without heating to dryness; (IV) with H 2 O 2 and with heating to dryness. In general, low recoveries of selenium are obtained for several marine species (e.g., crustaceans and cephalopods), which may be ascribed to the presence of Se forms mainly associated with nonpolar proteins and lipids. Post-digestion UV irradiation proved very efficient since not only complete organoselenium decomposition was achieved but also the final step required for prereduction of Se(VI) into Se(IV) (i.e. heating at 90 deg. C for 30 min in 6 M HCl) could be avoided. With the MAWD/UV procedure, the use of strong oxidising agents (persuphate, etc.) or acids (e.g. perchloric acid) which are typically applied prior to Se determination by hydride generation techniques is overcome, and as a result, sample pre-treatment is significantly simplified. The method was successfully validated against CRM DOLT-2 (dogfish liver), CRM DORM-2 (dogfish muscle) and CRM TORT-2 (lobster hepatopancreas). Automated ultrasonic slurry sampling with electrothermal atomic absorption spectrometry was also applied for comparison. Total Se contents in ten seafood samples were established. Se levels ranged from 0.7 to 2.9 μg g -1

A method for the complete analysis of NORM building materials by γ-ray spectrometry using HPGe detectors.

Science.gov (United States)

Quintana, B; Pedrosa, M C; Vázquez-Canelas, L; Santamaría, R; Sanjuán, M A; Puertas, F

2018-04-01

A methodology including software tools for analysing NORM building materials and residues by low-level gamma-ray spectrometry has been developed. It comprises deconvolution of gamma-ray spectra using the software GALEA with focus on the natural radionuclides and Monte Carlo simulations for efficiency and true coincidence summing corrections. The methodology has been tested on a range of building materials and validated against reference materials. Copyright © 2017 Elsevier Ltd. All rights reserved.

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

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.)

Development of gas ionization chambers with coplanar electrodes for alpha-ray spectrometry

International Nuclear Information System (INIS)

Iwasaki, Kenta; Tanaka, Naomichi; Murakami, Kohei; Hasebe, Nobuyuki; Kusano, Hiroki; Shibamura, Eido; Miyajima, Mitsuhiro

2016-01-01

A large-area alpha-ray spectrometer is required to measure the low level alpha emitters in environmental samples, which may be distributed in the vicinity of nuclear power plants. A gas ionization chamber with a coplanar electrode has attractive features such as with mechanical ruggedness, easy handling, easy fabrication of large electrode, and relatively well-known performance. We have investigated the performance of a gas ionization chamber with a coplanar electrode for alpha-ray spectrometry, particularly in the energy resolution. The present experiment shows that the energy resolution in the full width at half maximum (FWHM) is 129 keV (= 2.7%) for alpha-rays from Np with an energy of 4.78 MeV, 120 keV (= 2.2%) for those with 5.49 MeV from Am, and 109 keV (= 1.9%) for those with 5.81 MeV from Cm. It is found that the energy resolution obtained at the present experiment is dominated in the electronic noise caused by the large capacitance existed between the collecting anode (CA) and non-collecting anode (NCA) in the coplanar electrode. (author)

Affinity selection-mass spectrometry and its emerging application to the high throughput screening of G protein-coupled receptors.

Science.gov (United States)

Whitehurst, Charles E; Annis, D Allen

2008-07-01

Advances in combinatorial chemistry and genomics have inspired the development of novel affinity selection-based screening techniques that rely on mass spectrometry to identify compounds that preferentially bind to a protein target. Of the many affinity selection-mass spectrometry techniques so far documented, only a few solution-based implementations that separate target-ligand complexes away from unbound ligands persist today as routine high throughput screening platforms. Because affinity selection-mass spectrometry techniques do not rely on radioactive or fluorescent reporters or enzyme activities, they can complement traditional biochemical and cell-based screening assays and enable scientists to screen targets that may not be easily amenable to other methods. In addition, by employing mass spectrometry for ligand detection, these techniques enable high throughput screening of massive library collections of pooled compound mixtures, vastly increasing the chemical space that a target can encounter during screening. Of all drug targets, G protein coupled receptors yield the highest percentage of therapeutically effective drugs. In this manuscript, we present the emerging application of affinity selection-mass spectrometry to the high throughput screening of G protein coupled receptors. We also review how affinity selection-mass spectrometry can be used as an analytical tool to guide receptor purification, and further used after screening to characterize target-ligand binding interactions, enabling the classification of orthosteric and allosteric binders.

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

Remarks on the gamma-ray spectrometry for the determination of natural radioisotopes

International Nuclear Information System (INIS)

Kalita, S.; Niewodniczanski, J.

1987-01-01

Semiconductor low-energy gamma ray spectrometry is compared with the routinely used scintillation method (within higher energy range). Measurements of low-energy natural gamma radiation using a semiconductor detector permit the determination of radioactive equilibrium of the uranium series. In this method 238 U ( 234 Th) content is determined by 63 keV, 226 Ra by 186 keV and 214 Pb by 295 keV gamma rays. Using the same results one can calculate a radioactive equilibrium coefficient R, defined as concentration ratio 226 Ra/ 238 U and a 222 Rn emanation ratio E, defined as 1 - 214 Pb/ 226 Ra (concentrations in uranium equivalent units). The relative standard errors for the method are: 10 - 15% in case of radioisotope content and about 18% for R and E determination. 7 refs., 2 figs., 2 tabs. (author)

Analysis of total and dissolved heavy metals in surface water of a Mexican polluted river by total reflection X-ray fluorescence spectrometry

Energy Technology Data Exchange (ETDEWEB)

Zarazua, G. [Instituto Nacional de Investigaciones Nucleares, Gerencia de Ciencias Ambientales, Apartado Postal 18-1027, Mexico D.F., C.P. 11801 (Mexico)]. E-mail: gzo@nuclear.inin.mx; Avila-Perez, P. [Instituto Nacional de Investigaciones Nucleares, Gerencia de Ciencias Ambientales, Apartado Postal 18-1027, Mexico D.F., C.P. 11801 (Mexico); Tejeda, S. [Instituto Nacional de Investigaciones Nucleares, Gerencia de Ciencias Ambientales, Apartado Postal 18-1027, Mexico D.F., C.P. 11801 (Mexico); Barcelo-Quintal, I. [Universidad Autonoma Metropolitana, Unidad Azcapotzalco, Mexico, D.F. (Mexico); Martinez, T. [Universidad Nacional Autonoma de Mexico, Facultad de Quimica, Mexico, D.F. (Mexico)

2006-11-15

The present area of study is located in the Upper Course of the Lerma River (UCLR). The Lerma is one of the most important rivers of Mexico, where it drains highly populated and industrialized regions. The aim of the present study is to determine the heavy metal concentration of Cr, Mn, Fe, Cu and Pb in dissolved and total phases of the UCLR by means of Total Reflection X-ray Fluorescence Spectrometry (TXRF). The surface water samples were collected at 8 sites distributed following the stream flow direction of the river. Four sampling campaigns were carried out in each site in a 1-year period. A sample preparation method was applied in order to obtain the total and dissolved fraction and to destroy the organic matter. The total heavy metal average concentration decrease in the following order: Fe (2566 {mu}g/L) > Mn (300 {mu}g/L) > Cu (66 {mu}g/L) > Cr (21 {mu}g/L) > Pb (15 {mu}g/L). In general, the heavy metal concentrations in water of the UCLR are below the maximum permissible limits.

Analysis of total and dissolved heavy metals in surface water of a Mexican polluted river by total reflection X-ray fluorescence spectrometry

Science.gov (United States)

Zarazua, G.; Ávila-Pérez, P.; Tejeda, S.; Barcelo-Quintal, I.; Martínez, T.

2006-11-01

The present area of study is located in the Upper Course of the Lerma River (UCLR). The Lerma is one of the most important rivers of Mexico, where it drains highly populated and industrialized regions. The aim of the present study is to determine the heavy metal concentration of Cr, Mn, Fe, Cu and Pb in dissolved and total phases of the UCLR by means of Total Reflection X-ray Fluorescence Spectrometry (TXRF). The surface water samples were collected at 8 sites distributed following the stream flow direction of the river. Four sampling campaigns were carried out in each site in a 1-year period. A sample preparation method was applied in order to obtain the total and dissolved fraction and to destroy the organic matter. The total heavy metal average concentration decrease in the following order: Fe (2566 μg/L) > Mn (300 μg/L) > Cu (66 μg/L) > Cr (21 μg/L) > Pb (15 μg/L). In general, the heavy metal concentrations in water of the UCLR are below the maximum permissible limits.

Analysis of total and dissolved heavy metals in surface water of a Mexican polluted river by total reflection X-ray fluorescence spectrometry

International Nuclear Information System (INIS)

Zarazua, G.; Avila-Perez, P.; Tejeda, S.; Barcelo-Quintal, I.; Martinez, T.

2006-01-01

The present area of study is located in the Upper Course of the Lerma River (UCLR). The Lerma is one of the most important rivers of Mexico, where it drains highly populated and industrialized regions. The aim of the present study is to determine the heavy metal concentration of Cr, Mn, Fe, Cu and Pb in dissolved and total phases of the UCLR by means of Total Reflection X-ray Fluorescence Spectrometry (TXRF). The surface water samples were collected at 8 sites distributed following the stream flow direction of the river. Four sampling campaigns were carried out in each site in a 1-year period. A sample preparation method was applied in order to obtain the total and dissolved fraction and to destroy the organic matter. The total heavy metal average concentration decrease in the following order: Fe (2566 μg/L) > Mn (300 μg/L) > Cu (66 μg/L) > Cr (21 μg/L) > Pb (15 μg/L). In general, the heavy metal concentrations in water of the UCLR are below the maximum permissible limits

Radon gamma-ray spectrometry with YAP:Ce scintillator

CERN Document Server

Plastino, W; De Notaristefani, F

2002-01-01

The detection properties of a YAP:Ce scintillator (YAlO sub 3 :Ce crystal) optically coupled to a Hamamatsu H5784 photomultiplier with standard bialkali photocathode have been analyzed. In particular, the application to radon and radon-daughters gamma-ray spectrometry was investigated. The crystal response has been studied under severe extreme conditions to simulate environments of geophysical interest, particularly those found in geothermal and volcanic areas. Tests in water up to a temperature of 100 deg.C and in acids solutions such as HCl (37%), H sub 2 SO sub 4 (48%) and HNO sub 3 (65%) have been performed. The measurements with standard radon sources provided by the National Institute for Metrology of Ionizing Radiations (ENEA) have emphasized the non-hygroscopic properties of the scintillator and a small dependence of the light yield on temperature and HNO sub 3. The data collected in this first step of our research have pointed out that the YAP:Ce scintillator can allow high response stability for rad...

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

Mass spectrometry detection of G3m and IGHG3 alleles and follow-up of differential mother and neonate IgG3.

Directory of Open Access Journals (Sweden)

Célia Dechavanne

Full Text Available Mass spectrometry (MS analysis for detection of immunoglobulins (IG of the human IgG3 subclass is described that relies on polymorphic amino acids of the heavy gamma3 chains. IgG3 is the most polymorphic human IgG subclass with thirteen G3m allotypes located on the constant CH2 and CH3 domains of the gamma3 chain, the combination of which leads to six major G3m alleles. Amino acid changes resulting of extensive sequencing previously led to the definition of 19 IGHG3 alleles that have been correlated to the G3m alleles. As a proof of concept, MS proteotypic peptides were defined which encompass discriminatory amino acids for the identification of the G3m and IGHG3 alleles. Plasma samples originating from ten individuals either homozygous or heterozygous for different G3m alleles, and including one mother and her baby (drawn sequentially from birth to 9 months of age, were analyzed. Total IgG3 were purified using affinity chromatography and then digested by a combination of AspN and trypsin proteases, and peptides of interest were detected by mass spectrometry. The sensitivity of the method was assessed by mixing variable amounts of two plasma samples bearing distinct G3m allotypes. A label-free approach using the high-performance liquid chromatography (HPLC retention time of peptides and their MS mass analyzer peak intensity gave semi-quantitative information. Quantification was realized by selected reaction monitoring (SRM using synthetic peptides as internal standards. The possibility offered by this new methodology to detect and quantify neo-synthesized IgG in newborns will improve knowledge on the first acquisition of antibodies in infants and constitutes a promising diagnostic tool for vertically-transmitted diseases.

ICIT contribution to JET gamma-ray diagnostics enhancement

International Nuclear Information System (INIS)

Soare, S.; Curuia, M.; Zoita, V.

2010-01-01

Full text: Gamma-ray emission of tokamak plasmas is the result of the interaction of fast ions (fusion reaction products, including alpha particles, NBI ions, ICRH-accelerated ions) with main plasma impurities (e.g., carbon, beryllium). Gamma-ray diagnostics involve both gamma-ray imaging (cameras) and gamma-ray spectrometry (spectrometers). For the JET tokamak, gamma-ray diagnostics have been used to provide information on the characteristics of the fast ion population in plasmas. Two gamma-ray diagnostics enhancements project have been launched by JET and the MEdC/EURATOM Association has agreed to lead both of them with ICIT as projects leader. (authors)

Measurement of ²²⁶Ra in soil from oil field: advantages of γ-ray spectrometry and application to the IAEA-448 CRM.

Science.gov (United States)

Ceccatelli, A; Katona, R; Kis-Benedek, G; Pitois, A

2014-05-01

The analytical performance of gamma-ray spectrometry for the measurement of (226)Ra in TENORM (Technically Enhanced Naturally Occurring Radioactive Material) soil was investigated by the IAEA. Fast results were obtained for characterization and certification of a new TENORM Certified Reference Material (CRM), identified as IAEA-448 (soil from oil field). The combined standard uncertainty of the gamma-ray spectrometry results is of the order of 2-3% for massic activity measurement values ranging from 16500 Bq kg(-1) to 21500 Bq kg(-1). Methodologies used for the production and certification of the IAEA-448 CRM are presented. Analytical results were confirmed by alpha spectrometry. The "t" test showed agreement between alpha and gamma results at 95% confidence level. © 2013 Published by Elsevier Ltd.

Direct determination of trace elements in boron nitride powders by slurry sampling total reflection X-ray fluorescence spectrometry

International Nuclear Information System (INIS)

Amberger, Martin A.; Hoeltig, Michael; Broekaert, Jose A.C.

2010-01-01

The use of slurry sampling total reflection X-ray fluorescence spectrometry (SlS-TXRF) for the direct determination of Ca, Cr, Cu, Fe, Mn and Ti in four boron nitride powders has been described. Measurements of the zeta potential showed that slurries with good stabilities can be obtained by the addition of polyethylenimine (PEI) at a concentration of 0.1 wt.% and by adjusting the pH at 4. For the optimization of the concentration of boron nitride in the slurries the net line intensities and the signal to background ratios were determined for the trace elements Ca and Ti as well as for the internal standard element Ga in the case of concentrations of boron nitride ranging from 1 to 30 mg mL -1 . As a compromise with respect to high net line intensities and high signal to background ratios, concentrations of 5 mg mL -1 of boron nitride were found suitable and were used for all further measurements. The limits of detection of SlS-TXRF for the boron nitride powders were found to range from 0.062 to 1.6 μg g -1 for Cu and Ca, respectively. Herewith, they are higher than those obtained in solid sampling and slurry sampling graphite furnace atomic absorption spectrometry (SoS-GFAAS, SlS-GFAAS) as well as those of solid sampling electrothermal evaporation inductively coupled plasma optical emission spectrometry (SoS-ETV-ICP-OES). For Ca and Fe as well as for Cu and Fe, however, they were found to be lower than for GFAAS and for ICP-OES subsequent to wet chemical digestion, respectively. The universal applicability of SlS-TXRF to the analysis of samples with a wide variety of matrices could be demonstrated by the analysis of certified reference materials such as SiC, Al 2 O 3 , powdered bovine liver and borate ore with a single calibration. The correlation coefficients of the plots for the values found for Ca, Fe and Ti by SlS-TXRF in the boron nitride powders as well as in the before mentioned samples versus the reference values for the respective samples over a

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)

Specialised software utilities for gamma-ray spectrometry. Computer codes to IAEA-TECDOC-1275

International Nuclear Information System (INIS)

2002-03-01

A Co-ordinated Research Project (CRP) on 'Software Utilities for Gamma-Ray Spectrometry' was initiated by the International Atomic Energy Agency in 1996. In the CRP several basic applications of nuclear data handling were assayed which also dealt with the development of PC computer codes for various spectrometric purposes. This CD-ROM contains the following computer codes, produced under the CRP: ANGES, a program for the user controlled analysis of gamma-ray spectra from HPGe detectors; NUCL M AN, a program for the generation of gamma-ray libraries (using new, evaluated data) for specific applications; TRUE C OINC, a program to calculate true coincidence corrections; VOLUME, a program to calculate the full-energy peak efficiency calibration curve for homogeneous cylindrical sample geometries including self-attenuation correction; WINDIMEN, a program for the library driven analysis of gamma-ray spectra and for the quantification of radionuclide contents in the sample. RESFIT and DPPUNFOL, a set of programs for the definition of the detector resolution function and for unfolding of experimental annihilation spectra; MLMTEST, a program for the analysis of low-level NaI-spectra together with an extensive library of example reference spectra as well as a spectrum synthesizer

Near-optimum procedure for half-life measurement by high-resolution gamma-ray spectrometry

International Nuclear Information System (INIS)

Parker, J.L.

1989-01-01

A near-optimum procedure for using high-resolution γ-ray spectrometry to measure the half-lives of appropriate γ-ray- emitting-nuclides is presented. Among the important points of the procedure are the employment of the reference source method for implicit correction of pileup and deadtime losses; the use of full-energy peak-area ratios as the fundamental measured quantities; and continuous, high-rate data acquisition to obtain good results in a fraction of a half-life if desired. Equations are given for estimating the precision of the computed half-lives in terms of total measurement time, number of spectral acquisitions, and the precision of peak-area ratios. Results of 169 Yb half-life measurements are given as an example of the procedure's application. 3 refs., 2 tabs

Crystallization and preliminary X-ray analysis of Escherichia coli RNase G

International Nuclear Information System (INIS)

Fang, Pengfei; Wang, Jing; Li, Xu; Guo, Min; Xing, Li; Cao, Xu; Zhu, Yi; Gao, Yan; Niu, Liwen; Teng, Maikun

2009-01-01

Full-length E. coli RNase G was overexpressed, purified and crystallized. Diffraction data were collected to a resolution of 3.4 Å. The homologous RNases RNase E and RNase G are widely distributed in bacteria and function in many important physiological processes, including mRNA degradation, rRNA maturation and so on. In this study, the crystallization and preliminary X-ray analysis of RNase G from Escherichia coli is described. Purified recombinant E. coli RNase G, which has 497 amino acids, was crystallized in the cubic space group F432, with unit-cell parameters a = b = c = 219.84 Å. X-ray diffraction data were collected to a resolution of 3.4 Å

Development of an open source software of quantitative analysis for radionuclide determination by gamma-ray spectrometry using semiconductor detectors

International Nuclear Information System (INIS)

Maduar, Marcelo Francis

2010-01-01

Radioactivity quantification of gamma-ray emitter radionuclides in samples measured by HPGe gamma-ray spectrometry relies on the analysis of the photopeaks present in the spectra, especially on the accurate determination of their net areas. Such a task is usually performed with the aid of proprietary software tools. This work presents a methodology, algorithm descriptions and an open source application, called OpenGamma, for the peak search and analysis in order to obtain the relevant peaks parameters and radionuclides activities. The computational implementation is released entirely in open-source license for the main code and with the use of open software packages for interface design and mathematical libraries. The procedure for the peak search is performed on a three step approach. Firstly a preliminary search is done by using the second-difference method, consisting in the generation of a derived spectrum in order to find candidate peaks. In the second step, the experimental peaks widths are assessed and well formed and isolated ones are chosen to obtain a FWHM vs. channel relationship, by application of the Levenberg-Marquardt minimization method for non-linear fitting. Lastly, regions of the spectrum with grouped peaks are marked and a non-linear fit is again applied to each region to obtain baseline and photopeaks terms; from these terms, peaks net areas are then assessed. (author)

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

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

Nondestructive and quantitative characterization of TRU and LLW mixed-waste using active and passive gamma-ray spectrometry and computed tomography

Energy Technology Data Exchange (ETDEWEB)

Camp, D.C.; Martz, H.E.

1991-11-12

The technology being proposed by LLNL is an Active and Passive Computed Tomography (A P CT) Drum Scanner for contact-handled (CH) wastes. It combines the advantages offered by two well-developed nondestructive assay technologies: gamma-ray spectrometry and computed tomography (CT). Coupled together, these two technologies offer to nondestructively and quantitatively characterize mixed- wastes forms. Gamma-ray spectroscopy uses one or more external radiation detectors to passively and nondestructively measure the energy spectrum emitted from a closed container. From the resulting spectrum one can identify most radioactivities detected, be they transuranic isotopes, mixed-fission products, activation products or environmental radioactivities. Spectral libraries exist at LLNL for all four. Active (A) or transmission CT is a well-developed, nondestructive medical and industrial technique that uses an external-radiation beam to map regions of varying attenuation within a container. Passive (P) or emission CT is a technique mainly developed for medical application, e.g., single-photon emission CT. Nondestructive industrial uses of PCT are under development and just coming into use. This report discuses work on the A P CT Drum Scanner at LLNL.

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)

Reactor gamma spectrometry: status

International Nuclear Information System (INIS)

Gold, R.; Kaiser, B.J.

1979-01-01

Current work is described for Compton Recoil Gamma-Ray Spectrometry including developments in experimental technique as well as recent reactor spectrometry measurements. The current status of the method is described concerning gamma spectromoetry probe design and response characteristics. Emphasis is given to gamma spectrometry work in US LWR and BR programs. Gamma spectrometry in BR environments are outlined by focussing on start-up plans for the Fast Test Reactor (FTR). Gamma spectrometry results are presented for a LWR pressure vessel mockup in the Poolside Critical Assembly (PCA) at Oak Ridge National Laboratory

Comparison of in-situ gamma ray spectrometry measurements with conventional methods in determination natural and artificial nuclides in soil

International Nuclear Information System (INIS)

Al-Masri, M. S.; Doubal, A. W.

2010-12-01

Two nuclear analytical techniques (In-Situ Gamma ray spectrometry and laboratory gamma ray spectrometry) for determination of natural and artificial radionuclides in soil have been validated. The first technique depends on determination of radioactivity content of representative samples of the studied soil after laboratory preparation, while the second technique is based on direct determination of radioactivity content of soil using in-situ gamma-ray spectrometer. Analytical validation parameter such as detection limits, repeatability, reproducibility in addition to measurement uncertainties were estimated and compared for both techniques. Comparison results have shown that the determination of radioactivity in soil should apply the two techniques together where each of techniques is characterized by its low detection limit and uncertainty suitable for defined application of measurement. Radioactive isotopes in various locations were determined using the two methods by measuring 40 k, 238 U,and 137 Cs. The results showed that there are differences in attenuation factors due to soil moisture content differences; wet weight corrections should be applied when the two techniques are compared. (author)

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

Time-resolved and position-resolved X-ray spectrometry with a pixelated detector

Energy Technology Data Exchange (ETDEWEB)

Sievers, Peter

2012-12-07

The aim of the work presented here was to measure X-ray spectra with a pixelated detector. Due to effects in the sensor the spectrum cannot be measured directly and has to be calculated by a deconvolution of the measured data. In the scope of this work the deconvolution of the measured spectra could be enhanced considerably by - amongst other things - the introduction of the Bayesian deconvolution method. Those improvements opened the possibilities for further measurements. For the measurements the detectors of the Medipix family have been used. They are nowadays used for a wide range of applications and scientific research. Their main advantage is the very high position resolution gained by a pixel pitch of 55 μm and a high number of 65536 pixels. The Timepix detector has, in particular, two special possibilities of measurement: the ToA mode and the ToT mode. In ToA mode the arrival time of an impinging photon is measured and in ToT mode the amount of deposited charge is measured. The most common method of operation is counting the number of impinging photons that release a charge higher than a preset threshold in each pixel. As this released charge is proportional to the energy deposition of the impinging photon, one can perform energy-sensitive measurements. To perform the deconvolution of the measured energy distribution there is a need of an energy response matrix describing the detector response on radiation. For some detectors it is possible to obtain an analytic model of the response functions. Due to the high discrepancy between the impinging spectrum and the measured spectrum in case of detectors of the Medipix family, there is so far no analytic model. Thus, the detector response has to be simulated. As I could improve the precision of the measurement quite extensively, I also intended to tune the simulation with more accurate and appropriate models to gain the same level of accuracy. The results of measurement and simulation have then been compared and

Time-resolved and position-resolved X-ray spectrometry with a pixelated detector

International Nuclear Information System (INIS)

Sievers, Peter

2012-01-01

The aim of the work presented here was to measure X-ray spectra with a pixelated detector. Due to effects in the sensor the spectrum cannot be measured directly and has to be calculated by a deconvolution of the measured data. In the scope of this work the deconvolution of the measured spectra could be enhanced considerably by - amongst other things - the introduction of the Bayesian deconvolution method. Those improvements opened the possibilities for further measurements. For the measurements the detectors of the Medipix family have been used. They are nowadays used for a wide range of applications and scientific research. Their main advantage is the very high position resolution gained by a pixel pitch of 55 μm and a high number of 65536 pixels. The Timepix detector has, in particular, two special possibilities of measurement: the ToA mode and the ToT mode. In ToA mode the arrival time of an impinging photon is measured and in ToT mode the amount of deposited charge is measured. The most common method of operation is counting the number of impinging photons that release a charge higher than a preset threshold in each pixel. As this released charge is proportional to the energy deposition of the impinging photon, one can perform energy-sensitive measurements. To perform the deconvolution of the measured energy distribution there is a need of an energy response matrix describing the detector response on radiation. For some detectors it is possible to obtain an analytic model of the response functions. Due to the high discrepancy between the impinging spectrum and the measured spectrum in case of detectors of the Medipix family, there is so far no analytic model. Thus, the detector response has to be simulated. As I could improve the precision of the measurement quite extensively, I also intended to tune the simulation with more accurate and appropriate models to gain the same level of accuracy. The results of measurement and simulation have then been compared and

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

Energy Technology Data Exchange (ETDEWEB)

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

2013-07-15

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

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)

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

Accurate x-ray spectroscopy

International Nuclear Information System (INIS)

Deslattes, R.D.

1987-01-01

Heavy ion accelerators are the most flexible and readily accessible sources of highly charged ions. These having only one or two remaining electrons have spectra whose accurate measurement is of considerable theoretical significance. Certain features of ion production by accelerators tend to limit the accuracy which can be realized in measurement of these spectra. This report aims to provide background about spectroscopic limitations and discuss how accelerator operations may be selected to permit attaining intrinsically limited data

Sequencing Cyclic Peptides by Multistage Mass Spectrometry

Science.gov (United States)

Mohimani, Hosein; Yang, Yu-Liang; Liu, Wei-Ting; Hsieh, Pei-Wen; Dorrestein, Pieter C.; Pevzner, Pavel A.

2012-01-01

Some of the most effective antibiotics (e.g., Vancomycin and Daptomycin) are cyclic peptides produced by non-ribosomal biosynthetic pathways. While hundreds of biomedically important cyclic peptides have been sequenced, the computational techniques for sequencing cyclic peptides are still in their infancy. Previous methods for sequencing peptide antibiotics and other cyclic peptides are based on Nuclear Magnetic Resonance spectroscopy, and require large amount (miligrams) of purified materials that, for most compounds, are not possible to obtain. Recently, development of mass spectrometry based methods has provided some hope for accurate sequencing of cyclic peptides using picograms of materials. In this paper we develop a method for sequencing of cyclic peptides by multistage mass spectrometry, and show its advantages over single stage mass spectrometry. The method is tested on known and new cyclic peptides from Bacillus brevis, Dianthus superbus and Streptomyces griseus, as well as a new family of cyclic peptides produced by marine bacteria. PMID:21751357

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.

Rapid Classification and Identification of Multiple Microorganisms with Accurate Statistical Significance via High-Resolution Tandem Mass Spectrometry.

Science.gov (United States)

Alves, Gelio; Wang, Guanghui; Ogurtsov, Aleksey Y; Drake, Steven K; Gucek, Marjan; Sacks, David B; Yu, Yi-Kuo

2018-06-05

Rapid and accurate identification and classification of microorganisms is of paramount importance to public health and safety. With the advance of mass spectrometry (MS) technology, the speed of identification can be greatly improved. However, the increasing number of microbes sequenced is complicating correct microbial identification even in a simple sample due to the large number of candidates present. To properly untwine candidate microbes in samples containing one or more microbes, one needs to go beyond apparent morphology or simple "fingerprinting"; to correctly prioritize the candidate microbes, one needs to have accurate statistical significance in microbial identification. We meet these challenges by using peptide-centric representations of microbes to better separate them and by augmenting our earlier analysis method that yields accurate statistical significance. Here, we present an updated analysis workflow that uses tandem MS (MS/MS) spectra for microbial identification or classification. We have demonstrated, using 226 MS/MS publicly available data files (each containing from 2500 to nearly 100,000 MS/MS spectra) and 4000 additional MS/MS data files, that the updated workflow can correctly identify multiple microbes at the genus and often the species level for samples containing more than one microbe. We have also shown that the proposed workflow computes accurate statistical significances, i.e., E values for identified peptides and unified E values for identified microbes. Our updated analysis workflow MiCId, a freely available software for Microorganism Classification and Identification, is available for download at https://www.ncbi.nlm.nih.gov/CBBresearch/Yu/downloads.html . Graphical Abstract ᅟ.

Screening and confirmation criteria for hormone residue analysis using liquid chromatography accurate mass time-of-flight, Fourier transform ion cyclotron resonance and orbitrap mass spectrometry techniques

NARCIS (Netherlands)

Nielen, M.W.F.; Engelen, M.C. van; Zuiderent, R.; Ramaker, R.

2007-01-01

An emerging trend is recognised in hormone and veterinary drug residue analysis from liquid chromatography tandem mass spectrometry (LC/MS/MS) based screening and confirmation towards accurate mass alternatives such as LC coupled with time-of-flight (TOF), Fourier transform ion cyclotron resonance

Simulation of single grid-based phase-contrast x-ray imaging (g-PCXI)

Energy Technology Data Exchange (ETDEWEB)

Lim, H.W.; Lee, H.W. [Department of Radiation Convergence Engineering, iTOMO Group, Yonsei University, 1 Yonseidae-gil, Wonju, Gangwon-do 26493 (Korea, Republic of); Cho, H.S., E-mail: hscho1@yonsei.ac.kr [Department of Radiation Convergence Engineering, iTOMO Group, Yonsei University, 1 Yonseidae-gil, Wonju, Gangwon-do 26493 (Korea, Republic of); Je, U.K.; Park, C.K.; Kim, K.S.; Kim, G.A.; Park, S.Y.; Lee, D.Y.; Park, Y.O.; Woo, T.H. [Department of Radiation Convergence Engineering, iTOMO Group, Yonsei University, 1 Yonseidae-gil, Wonju, Gangwon-do 26493 (Korea, Republic of); Lee, S.H.; Chung, W.H.; Kim, J.W.; Kim, J.G. [R& D Center, JPI Healthcare Co., Ltd., Ansan 425-833 (Korea, Republic of)

2017-04-01

Single grid-based phase-contrast x-ray imaging (g-PCXI) technique, which was recently proposed by Wen et al. to retrieve absorption, scattering, and phase-gradient images from the raw image of the examined object, seems a practical method for phase-contrast imaging with great simplicity and minimal requirements on the setup alignment. In this work, we developed a useful simulation platform for g-PCXI and performed a simulation to demonstrate its viability. We also established a table-top setup for g-PCXI which consists of a focused-linear grid (200-lines/in strip density), an x-ray tube (100-μm focal spot size), and a flat-panel detector (48-μm pixel size) and performed a preliminary experiment with some samples to show the performance of the simulation platform. We successfully obtained phase-contrast x-ray images of much enhanced contrast from both the simulation and experiment and the simulated contract seemed similar to the experimental contrast, which shows the performance of the developed simulation platform. We expect that the simulation platform will be useful for designing an optimal g-PCXI system. - Highlights: • It is proposed for the single grid-based phase-contrast x-ray imaging (g-PCXI) technique. • We implemented for a numerical simulation code. • The preliminary experiment with several samples to compare is performed. • It is expected to be useful to design an optimal g-PCXI system.

Determination of As concentration in earthworm coelomic fluid extracts by total-reflection X-ray fluorescence spectrometry

Science.gov (United States)

Allegretta, Ignazio; Porfido, Carlo; Panzarino, Onofrio; Fontanella, Maria Chiara; Beone, Gian Maria; Spagnuolo, Matteo; Terzano, Roberto

2017-04-01

Earthworms are often used as sentinel organisms to study As bioavailability in polluted soils. Arsenic in earthworms is mainly sequestrated in the coelomic fluids whose As content can therefore be used to asses As bioavalability. In this work, a method for determining As concentration in coelomic fluid extracts using total-reflection X-ray fluorescence spectrometry (TXRF) is presented. For this purpose coelomic fluid extracts from earthworms living in three polluted soils and one non-polluted (control) soil have been collected and analysed. A very simple sample preparation was implemented, consisting of a dilution of the extracts with polyvinyl alcohol (PVA) using a 1:8 ratio and dropwise deposition of the sample on the reflector. A detection limit of 0.2 μg/l and quantification limit of 0.6 μg/l was obtained in the diluted samples, corresponding to 2 μg/l and 6 μg/l in the coelomic fluid extracts, respectively. This allowed to quantify As concentration in coelomic fluids extracted from earthworms living in soils polluted with As at concentrations higher than 20 mg/kg (considered as a pollution threshold for agricultural soils). The TXRF method has been validated by comparison with As concentrations in standards and by analysing the same samples by ICP-MS, after acid digestion of the sample. The low limit of detection, the proven reliability of the method and the little sample preparation make TXRF a suitable, cost-efficient and "green" technique for the analysis of As in earthworm coelomic fluid extracts for bioavailability studies.

Shaly sand evaluation using gamma ray spectrometry, applied to the North Sea Jurassic

International Nuclear Information System (INIS)

Marett, G.; Chevalier, P.; Souhaite, P.; Suau, J.

1976-01-01

In formations where radioactive minerals other than clay are present, their effects on log responses result in a reduction of the accuracy of determination of the shale fraction. The gamma ray log, which is one of the primary indicators for shaliness determination, is the most affected; other logs used in shaliness indicators are also influenced, particularly when heavy minerals are present, such as those encountered in the micaceous sandstones of the North Sea Jurassic. For comparison purposes, possible ways to correct for heavy radioactive minerals using a conventional logging suite are described. Computer processed examples illustrate the results obtained. A different approach is through an analysis of the natural gamma ray spectrum of the formation, as determined with the gamma ray spectrometry tool. Natural gamma rays originate from the radioactive isotope of potassium and the radioactive elements of the uranium and thorium series. Each of these three elements contributes its distinctive spectrum to that of the formation in proportion to its abundance. Thus, by analysis of the formation spectrum, the presence of each can be detected and its amount estimated. This makes possible quantitative corrections to the shaliness indicators. A computer program which performs the necessary computations is described, and several log examples using this technique are presented

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.

Standard test method for quantitative determination of americium 241 in plutonium by Gamma-Ray spectrometry

CERN Document Server

American Society for Testing and Materials. Philadelphia

1994-01-01

1.1 This test method covers the quantitative determination of americium 241 by gamma-ray spectrometry in plutonium nitrate solution samples that do not contain significant amounts of radioactive fission products or other high specific activity gamma-ray emitters. 1.2 This test method can be used to determine the americium 241 in samples of plutonium metal, oxide and other solid forms, when the solid is appropriately sampled and dissolved. 1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

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.

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.

Mapping the spatial distribution and activity of "2"2"6Ra at legacy sites through Machine Learning interpretation of gamma-ray spectrometry data

International Nuclear Information System (INIS)

Varley, Adam; Tyler, Andrew; Smith, Leslie; Dale, Paul; Davies, Mike

2016-01-01

Radium ("2"2"6Ra) contamination derived from military, industrial, and pharmaceutical products can be found at a number of historical sites across the world posing a risk to human health. The analysis of spectral data derived using gamma-ray spectrometry can offer a powerful tool to rapidly estimate and map the activity, depth, and lateral distribution of "2"2"6Ra contamination covering an extensive area. Subsequently, reliable risk assessments can be developed for individual sites in a fraction of the timeframe compared to traditional labour-intensive sampling techniques: for example soil coring. However, local heterogeneity of the natural background, statistical counting uncertainty, and non-linear source response are confounding problems associated with gamma-ray spectral analysis. This is particularly challenging, when attempting to deal with enhanced concentrations of a naturally occurring radionuclide such as "2"2"6Ra. As a result, conventional surveys tend to attribute the highest activities to the largest total signal received by a detector (Gross counts): an assumption that tends to neglect higher activities at depth. To overcome these limitations, a methodology was developed making use of Monte Carlo simulations, Principal Component Analysis and Machine Learning based algorithms to derive depth and activity estimates for "2"2"6Ra contamination. The approach was applied on spectra taken using two gamma-ray detectors (Lanthanum Bromide and Sodium Iodide), with the aim of identifying an optimised combination of detector and spectral processing routine. It was confirmed that, through a combination of Neural Networks and Lanthanum Bromide, the most accurate depth and activity estimates could be found. The advantage of the method was demonstrated by mapping depth and activity estimates at a case study site in Scotland. There the method identified significantly higher activity ( 0.4 m), that conventional gross counting algorithms failed to identify. It was

An improved in situ method for determining depth distributions of gamma-ray emitting radionuclides

International Nuclear Information System (INIS)

Benke, R.R.; Kearfott, K.J.

2001-01-01

In situ gamma-ray spectrometry determines the quantities of radionuclides in some medium with a portable detector. The main limitation of in situ gamma-ray spectrometry lies in determining the depth distribution of radionuclides. This limitation is addressed by developing an improved in situ method for determining the depth distributions of gamma-ray emitting radionuclides in large area sources. This paper implements a unique collimator design with conventional radiation detection equipment. Cylindrically symmetric collimators were fabricated to allow only those gamma-rays emitted from a selected range of polar angles (measured off the detector axis) to be detected. Positioned with its axis normal to surface of the media, each collimator enables the detection of gamma-rays emitted from a different range of polar angles and preferential depths. Previous in situ methods require a priori knowledge of the depth distribution shape. However, the absolute method presented in this paper determines the depth distribution as a histogram and does not rely on such assumptions. Other advantages over previous in situ methods are that this method only requires a single gamma-ray emission, provides more detailed depth information, and offers a superior ability for characterizing complex depth distributions. Collimated spectrometer measurements of buried area sources demonstrated the ability of the method to yield accurate depth information. Based on the results of actual measurements, this method increases the potential of in situ gamma-ray spectrometry as an independent characterization tool in situations with unknown radionuclide depth distributions

Gamma-ray spectrometry combined with acceptable knowledge (GSAK). A technique for characterization of certain remote-handled transuranic (RH-TRU) wastes. Part 1. Methodology and techniques

International Nuclear Information System (INIS)

Hartwell, J.K.; McIlwain, M.E.

2005-01-01

Gamma-ray spectrometry combined with acceptable knowledge (GSAK) is a technique for the characterization of certain remote-handled transuranic (RH-TRU) wastes. GSAK uses gamma-ray spectrometry to quantify a portion of the fission product inventory of RH-TRU wastes. These fission product results are then coupled with calculated inventories derived from acceptable process knowledge to characterize the radionuclide content of the assayed wastes. GSAK has been evaluated and tested through several test exercises. GSAK approach is described, while test results are presented in Part II. (author)

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

Energy Technology Data Exchange (ETDEWEB)

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

2016-12-15

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

Tomosynthesis can facilitate accurate measurement of joint space width under the condition of the oblique incidence of X-rays in patients with rheumatoid arthritis.

Science.gov (United States)

Ono, Yohei; Kashihara, Rina; Yasojima, Nobutoshi; Kasahara, Hideki; Shimizu, Yuka; Tamura, Kenichi; Tsutsumi, Kaori; Sutherland, Kenneth; Koike, Takao; Kamishima, Tamotsu

2016-06-01

Accurate evaluation of joint space width (JSW) is important in the assessment of rheumatoid arthritis (RA). In clinical radiography of bilateral hands, the oblique incidence of X-rays is unavoidable, which may cause perceptional or measurement error of JSW. The objective of this study was to examine whether tomosynthesis, a recently developed modality, can facilitate a more accurate evaluation of JSW than radiography under the condition of oblique incidence of X-rays. We investigated quantitative errors derived from the oblique incidence of X-rays by imaging phantoms simulating various finger joint spaces using radiographs and tomosynthesis images. We then compared the qualitative results of the modified total Sharp score of a total of 320 joints from 20 patients with RA between these modalities. A quantitative error was prominent when the location of the phantom was shifted along the JSW direction. Modified total Sharp scores of tomosynthesis images were significantly higher than those of radiography, that is to say JSW was regarded as narrower in tomosynthesis than in radiography when finger joints were located where the oblique incidence of X-rays is expected in the JSW direction. Tomosynthesis can facilitate accurate evaluation of JSW in finger joints of patients with RA, even with oblique incidence of X-rays. Accurate evaluation of JSW is necessary for the management of patients with RA. Through phantom and clinical studies, we demonstrate that tomosynthesis may achieve more accurate evaluation of JSW.

Rapid analysis of 226Ra in mine waters by gamma-ray spectrometry. Supervising Scientist report 103

International Nuclear Information System (INIS)

Johnston, A.; Martin, P.

1995-01-01

Techniques for the determination of 226 Ra in uranium mine waters by γ-ray spectrometry are examined with an emphasis on methods capable of completion within 1 to 3 days of receipt of the sample. Methods discussed utilise either: (i) the 186 keV 226 Ra γ-ray, with the contribution from 235 U being subtracted after a separate uranium determination, or (ii) measurement of ingrowing 222 Rn progeny, either by two successive counts or by a single count (together with an assumption that radon was not present at the time of sample preparation). A full analysis of the statistical uncertainties and systematic errors associated with each technique is presented

Accurate determination and certification of bromine in plastic by isotope dilution inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Ohata, Masaki; Miura, Tsutomu

2014-01-01

Highlights: • Accurate analytical method of Br in plastic was studied by isotope dilution ICPMS. • A microwave acid digestion using quartz vessel was suitable for Br analysis. • Sample dilution by NH 3 solution could remove memory effect for ICPMS measurement. • The analytical result of the ID-ICPMS showed consistency with that of INAA. • The ID-ICPMS developed could apply to certification of Br in candidate plastic CRM. - Abstract: The accurate analytical method of bromine (Br) in plastic was developed by an isotope dilution inductively coupled plasma mass spectrometry (ID-ICPMS). The figures of merit of microwave acid digestion procedures using polytetrafluoroethylene (PTFE) or quartz vessels were studied and the latter one was suitable for Br analysis since its material was free from Br contamination. The sample dilution procedures using Milli-Q water or ammonium (NH 3 ) solution were also studied to remove memory effect for ICPMS measurement. Although severe memory effect was observed on Milli-Q water dilution, NH 3 solution could remove it successfully. The accuracy of the ID-ICPMS was validated by a certified reference material (CRM) as well as the comparison with the analytical result obtained by an instrumental neutron activation analysis (INAA) as different analytical method. From these results, the ID-ICPMS developed in the present study could be evaluated as accurate analytical method of Br in plastic materials and it could apply to certification of Br in candidate plastic CRM with respect to such regulations related to RoHS (restriction of the use of hazardous substances in electrical and electronics equipment) directive

The determination of lead, zinc, and magnesium in dolomite and its benefication products by use of x-ray-fluorescence spectrometry

International Nuclear Information System (INIS)

Jacobs, J.J.

1985-01-01

An investigation was undertaken on the development of fast, simple, and accurate methods of analysis for lead and zinc in tailings and middlings from dolomite, and for lead, zinc, and magnesium in concentrates obtained from dolomite. A pressed-powder technique and X-ray-fluorescence spectrometry (XRFS) were used. Good agreement was found between the XRFS values for lead and zinc in low concentrations and the values obtained by other techniques of analysis when the calibration for the XRFS method was effected by the use of synthetic standards comprising lead and zinc oxides in a dolomite matrix. For high concentrations of the analytes, all the oxides and sulphides of lead and zinc in the samples had to be converted to the sulphate form, and a matrix correction had to be applied to the assigned values of the oxide calibration standards. The lower limits of detection for lead, zinc, and magnesium were 0,004, 0,003, and 0,18 per cent respectively. The recommended methods are detailed in two appendices

Monitoring of blood-10B concentration for boron neutron capture therapy using prompt gamma-ray analysis

International Nuclear Information System (INIS)

Raaijmakers, C.P.J.; Konijnenberg, M.W.; Dewit, L.; Mijnheer, B.J.; Haritz, D.; Huiskamp, R.; Philipp, K.; Siefert, A.; Stecher-Rasmussen, F.

1995-01-01

The aim of the present study was to monitor the blood- 10 B concentration of laboratory dogs receiving boron neutron capture therapy, in order to obtain optimal agreement between prescribed and actual dose. A prompt gamma-ray analysis system was developed for this purpose at the High Flux Reactor in Petten. The technique was compared with inductively coupled plasma-atomic emission spectrometry and showed good agreement. A substantial variation in 10 B clearance pattern after administration of borocaptate sodium was found between the different dogs. Consequently, the irradiation commencement was adjusted to the individually determined boron elimination curve. Mean blood- 10 B concentratios during irradiation of 25.8±2.2 μg/g (1 SD, n=18) and 49.3±5.3 μg/g (1 SD, n=17) were obtained for intended concentrations of 25 μg/g and 50 μg/g, respectively. These variations are a factor of two smaller than irradiations performed at a uniform post-infusion irradiation starting time. Such a careful bolld- 10 B monitoring procedure is a prerequisite for accurately obtaining such steep dose-response curves as observed during the dog study. (orig.)

Gamma-ray spectrometry combined with acceptable knowledge (GSAK). A technique for characterization of certain remote-handled transuranic (RH-TRU) wastes. Part 2. Testing and results

International Nuclear Information System (INIS)

Hartwell, J.K.; McIlwain, M.E.

2005-01-01

Gamma-ray spectrometry combined with acceptable knowledge (GSAK) is a technique for the characterization of certain remote-handled transuranic (RH-TRU) wastes. GSAK uses gamma-ray spectrometry to quantify a portion of the fission product inventory of RH-TRU wastes. These fission product results are then coupled with calculated inventories derived from acceptable process knowledge to characterize the radionuclide content of the assayed wastes. GSAK has been evaluated and tested through several test exercises. These tests and their results are described; while the former paper in this issue presents the methodology, equipment and techniques. (author)

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)

Survey of natural radioactivity levels in Ilex paraguariensis (St. Hil.) by gamma-ray spectrometry

International Nuclear Information System (INIS)

Scheibel, Viviane; Appoloni, Carlos Roberto

2007-01-01

The mate tea (Ilex paraguariensis - St. Hil.) is a beverage broadly cultivated and consumed in Brazil. The radioactive traces present in three trademarks of toasted mate tea produced at the south of Brazil were analyzed. Measurements were carried out by gamma-ray spectrometry. The average value for the 40 K activity measured for marks A, B and C was 1216 ± 8, 1047 ± 14 and 666 ± 13 Bq.kg -1 , respectively. The 137 Cs activity was lower than the limit of detection. (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.

Simultaneous determination of actinides by x-ray fluorescence spectrometry

International Nuclear Information System (INIS)

Cohen, V.H.

1990-01-01

The x-ray spectrometric simultaneous determination of uranium and plutonium in simulated Purex Process solutions is described. The method is accomplished by intensity measurements of the L α sub(1) lines. The thin film technique for sample preparation and thorium as an internal standard had been used. An evaporation technique had been also tested for low concentration uranium solutions. In the measurement range 0,05 - 130 U g/L, 0,5 - 20 Pu g/L linear calibration curves were effected. The standard deviation in the concentration range 10 to 130 g/L was 3,5%, 4% in the 1 to 10 g/L and 13% in 0,05 to 1 g/L for uranium determination and 4% for plutonium determination in the range of 1 to 20 g/L. The sensitivity of the method was about 3,62 μg to U and 3,95 μg to Pu. Uranium and plutonium do not reciprocally interfere with one another until U/Pu ≅ 90 m/m. The fission product as interfering elements were also verified. Finally, uranium and plutonium were determined in simulated Purex Process solutions within the requested accuracy for control method. (author)

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)

Evaluation of a new optic-enabled portable X-ray fluorescence spectrometry instrument for measuring toxic metals/metalloids in consumer goods and cultural products

Science.gov (United States)

Guimarães, Diana; Praamsma, Meredith L.; Parsons, Patrick J.

2016-08-01

X-ray fluorescence spectrometry (XRF) is a rapid, non-destructive multi-elemental analytical technique used for determining elemental contents ranging from percent down to the μg/g level. Although detection limits are much higher for XRF compared to other laboratory-based methods, such as inductively coupled plasma mass spectrometry (ICP-MS), ICP-optical emission spectrometry (OES) and atomic absorption spectrometry (AAS), its portability and ease of use make it a valuable tool, especially for field-based studies. A growing necessity to monitor human exposure to toxic metals and metalloids in consumer goods, cultural products, foods and other sample types while performing the analysis in situ has led to several important developments in portable XRF technology. In this study, a new portable XRF analyzer based on the use of doubly curved crystal optics (HD Mobile®) was evaluated for detecting toxic elements in foods, medicines, cosmetics and spices used in many Asian communities. Two models of the HD Mobile® (a pre-production and a final production unit) were investigated. Performance parameters including accuracy, precision and detection limits were characterized in a laboratory setting using certified reference materials (CRMs) and standard solutions. Bias estimates for key elements of public health significance such as As, Cd, Hg and Pb ranged from - 10% to 11% for the pre-production, and - 14% to 16% for the final production model. Five archived public health samples including herbal medicine products, ethnic spices and cosmetic products were analyzed using both XRF instruments. There was good agreement between the pre-production and final production models for the four key elements, such that the data were judged to be fit-for-purpose for the majority of samples analyzed. Detection of the four key elements of interest using the HD Mobile® was confirmed using archived samples for which ICP-OES data were available based on digested sample materials. The HD

Nondestructive and quantitative characterization of TRU and LLW mixed-waste using active and passive gamma-ray spectrometry and computed tomography

International Nuclear Information System (INIS)

Camp, D.C.; Martz, H.E.

1991-01-01

The technology being proposed by LLNL is an Active and Passive Computed Tomography (A ampersand P CT) Drum Scanner for contact-handled (CH) wastes. It combines the advantages offered by two well-developed nondestructive assay technologies: gamma-ray spectrometry and computed tomography (CT). Coupled together, these two technologies offer to nondestructively and quantitatively characterize mixed- wastes forms. Gamma-ray spectroscopy uses one or more external radiation detectors to passively and nondestructively measure the energy spectrum emitted from a closed container. From the resulting spectrum one can identify most radioactivities detected, be they transuranic isotopes, mixed-fission products, activation products or environmental radioactivities. Spectral libraries exist at LLNL for all four. Active (A) or transmission CT is a well-developed, nondestructive medical and industrial technique that uses an external-radiation beam to map regions of varying attenuation within a container. Passive (P) or emission CT is a technique mainly developed for medical application, e.g., single-photon emission CT. Nondestructive industrial uses of PCT are under development and just coming into use. This report discuses work on the A ampersand P CT Drum Scanner at LLNL

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...

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

On-line interrogation of pebble bed reactor fuel using passive gamma-ray spectrometry

Science.gov (United States)

Chen, Jianwei

The Pebble Bed Reactor (PBR) is a helium-cooled, graphite-moderated high temperature nuclear power reactor. In addition to its inherently safe design, a unique feature of this reactor is its multipass fuel cycle in which graphite fuel pebbles (of varying enrichment) are randomly loaded and continuously circulated through the core until they reach their prescribed end-of-life burnup limit (˜80,000--100,000 MWD/MTU). Unlike the situation with conventional light water reactors (LWRs), depending solely on computational methods to perform in-core fuel management will be highly inaccurate. As a result, an on-line measurement approach becomes the only accurate method to assess whether a particular pebble has reached its end-of-life burnup limit. In this work, an investigation was performed to assess the feasibility of passive gamma-ray spectrometry assay as an approach for on-line interrogation of PBR fuel for the simultaneous determination of burnup and enrichment on a pebble-by-pebble basis. Due to the unavailability of irradiated or fresh pebbles, Monte Carlo simulations were used to study the gamma-ray spectra of the PBR fuel at various levels of burnup. A pebble depletion calculation was performed using the ORIGEN code, which yielded the gamma-ray source term that was introduced into the input of an MCNP simulation. The MCNP simulation assumed the use of a high-purity coaxial germanium detector. Due to the lack of one-group high temperature reactor cross sections for ORIGEN, a heterogeneous MCNP model was developed to describe a typical PBR core. Subsequently, the code MONTEBURNS was used to couple the MCNP model and ORIGEN. This approach allowed the development of the burnup-dependent, one-group spectral-averaged PBR cross sections to be used in the ORIGEN pebble depletion calculation. Based on the above studies, a relative approach for performing the measurements was established. The approach is based on using the relative activities of Np-239/I-132 in combination

Accurate screening for synthetic preservatives in beverage using high performance liquid chromatography with time-of-flight mass spectrometry

International Nuclear Information System (INIS)

Li Xiuqin; Zhang Feng; Sun Yanyan; Yong Wei; Chu Xiaogang; Fang Yanyan; Zweigenbaum, Jerry

2008-01-01

In this study, liquid chromatography time-of-flight mass spectrometry (HPLC/TOF-MS) is applied to qualitation and quantitation of 18 synthetic preservatives in beverage. The identification by HPLC/TOF-MS is accomplished with the accurate mass (the subsequent generated empirical formula) of the protonated molecules [M + H]+ or the deprotonated molecules [M - H]-, along with the accurate mass of their main fragment ions. In order to obtain sufficient sensitivity for quantitation purposes (using the protonated or deprotonated molecule) and additional qualitative mass spectrum information provided by the fragments ions, segment program of fragmentor voltages is designed in positive and negative ion mode, respectively. Accurate mass measurements are highly useful in the complex sample analyses since they allow us to achieve a high degree of specificity, often needed when other interferents are present in the matrix. The mass accuracy typically obtained is routinely better than 3 ppm. The 18 compounds behave linearly in the 0.005-5.0 mg.kg -1 concentration range, with correlation coefficient >0.996. The recoveries at the tested concentrations of 1.0 mg.kg -1 -100 mg.kg -1 are 81-106%, with coefficients of variation -1 , which are far below the required maximum residue level (MRL) for these preservatives in foodstuff. The method is suitable for routine quantitative and qualitative analyses of synthetic preservatives in foodstuff

Research on digital airborne gamma-ray spectrometry

International Nuclear Information System (INIS)

Ge Liangquan; Lai Wanchang; Zeng Guoqiang; Fan Zhenguo; Xiong Shengqing; Ni Weizhong

2010-01-01

Airborne Gamma-ray Spectrometry (AGS) is a main supporting technique for looking for uranium deposits and other non-radioactive mineral deposit, as well as for investigating environmental radiation pollution and monitoring nuclear equipment. This paper describes the newest achievements about the AGS instrument developed by Chengdu university of Technology. Those are: 1) the probe of AGS is composed of 5 NaI(Tl) + PMT scintillation counters with 10 x 10 x 40 mm size, and a special temperature sensor, preamplifier with circuit negative feedback and high voltage with lower electronic noise have been designed. 2)A Y/U double channel digital controlled gain amplifier for adjusting the spectrum drift finely and high speed ADC and CPLD are designed to perform digitalized spectroscopy and to improve the energy resolution and pulse through output rate (more than 100k/s). 3) Two self-stabilization spectrum loops have been designed for spectrum stability: The first loop is roughly adjusted by temperature and the second loop is finely by Kalman filter. 4) The significant characters of new AGS system are: the detective gamma energy range is 0.02∼10.0 MeV, the spectrum drift is ±1 channel, the collecting period is 0.5-1 s, and 20 NaI(Tl)+PMT scintillation counters can be operated at the same time. (authors)

Introducing GAMER: A Fast and Accurate Method for Ray-tracing Galaxies Using Procedural Noise

Science.gov (United States)

Groeneboom, N. E.; Dahle, H.

2014-03-01

We developed a novel approach for fast and accurate ray-tracing of galaxies using procedural noise fields. Our method allows for efficient and realistic rendering of synthetic galaxy morphologies, where individual components such as the bulge, disk, stars, and dust can be synthesized in different wavelengths. These components follow empirically motivated overall intensity profiles but contain an additional procedural noise component that gives rise to complex natural patterns that mimic interstellar dust and star-forming regions. These patterns produce more realistic-looking galaxy images than using analytical expressions alone. The method is fully parallelized and creates accurate high- and low- resolution images that can be used, for example, in codes simulating strong and weak gravitational lensing. In addition to having a user-friendly graphical user interface, the C++ software package GAMER is easy to implement into an existing code.

Introducing GAMER: A fast and accurate method for ray-tracing galaxies using procedural noise

International Nuclear Information System (INIS)

Groeneboom, N. E.; Dahle, H.

2014-01-01

We developed a novel approach for fast and accurate ray-tracing of galaxies using procedural noise fields. Our method allows for efficient and realistic rendering of synthetic galaxy morphologies, where individual components such as the bulge, disk, stars, and dust can be synthesized in different wavelengths. These components follow empirically motivated overall intensity profiles but contain an additional procedural noise component that gives rise to complex natural patterns that mimic interstellar dust and star-forming regions. These patterns produce more realistic-looking galaxy images than using analytical expressions alone. The method is fully parallelized and creates accurate high- and low- resolution images that can be used, for example, in codes simulating strong and weak gravitational lensing. In addition to having a user-friendly graphical user interface, the C++ software package GAMER is easy to implement into an existing code.

Introducing GAMER: A fast and accurate method for ray-tracing galaxies using procedural noise

Energy Technology Data Exchange (ETDEWEB)

Groeneboom, N. E.; Dahle, H., E-mail: nicolaag@astro.uio.no [Institute of Theoretical Astrophysics, University of Oslo, P.O. Box 1029 Blindern, N-0315 Oslo (Norway)

2014-03-10

We developed a novel approach for fast and accurate ray-tracing of galaxies using procedural noise fields. Our method allows for efficient and realistic rendering of synthetic galaxy morphologies, where individual components such as the bulge, disk, stars, and dust can be synthesized in different wavelengths. These components follow empirically motivated overall intensity profiles but contain an additional procedural noise component that gives rise to complex natural patterns that mimic interstellar dust and star-forming regions. These patterns produce more realistic-looking galaxy images than using analytical expressions alone. The method is fully parallelized and creates accurate high- and low- resolution images that can be used, for example, in codes simulating strong and weak gravitational lensing. In addition to having a user-friendly graphical user interface, the C++ software package GAMER is easy to implement into an existing code.

AtomDB: Expanding an Accessible and Accurate Atomic Database for X-ray Astronomy

Science.gov (United States)

Smith, Randall

Since its inception in 2001, the AtomDB has become the standard repository of accurate and accessible atomic data for the X-ray astrophysics community, including laboratory astrophysicists, observers, and modelers. Modern calculations of collisional excitation rates now exist - and are in AtomDB - for all abundant ions in a hot plasma. AtomDB has expanded beyond providing just a collisional model, and now also contains photoionization data from XSTAR as well as a charge exchange model, amongst others. However, building and maintaining an accurate and complete database that can fully exploit the diagnostic potential of high-resolution X-ray spectra requires further work. The Hitomi results, sadly limited as they were, demonstrated the urgent need for the best possible wavelength and rate data, not merely for the strongest lines but for the diagnostic features that may have 1% or less of the flux of the strong lines. In particular, incorporation of weak but powerfully diagnostic satellite lines will be crucial to understanding the spectra expected from upcoming deep observations with Chandra and XMM-Newton, as well as the XARM and Athena satellites. Beyond incorporating this new data, a number of groups, both experimental and theoretical, have begun to produce data with errors and/or sensitivity estimates. We plan to use this to create statistically meaningful spectral errors on collisional plasmas, providing practical uncertainties together with model spectra. We propose to continue to (1) engage the X-ray astrophysics community regarding their issues and needs, notably by a critical comparison with other related databases and tools, (2) enhance AtomDB to incorporate a large number of satellite lines as well as updated wavelengths with error estimates, (3) continue to update the AtomDB with the latest calculations and laboratory measurements, in particular velocity-dependent charge exchange rates, and (4) enhance existing tools, and create new ones as needed to

Gamma spectrometry of infinite 4Π geometry

International Nuclear Information System (INIS)

Nordemann, D.J.R.

1987-07-01

Owing to the weak absorption og gamma radiation by matter, gamma-ray spectrometry may be applied to samples of great volume. A very interesting case is that of the gamma-ray spectrometry applied with 4Π geometry around the detector on a sample assumed to be of infinite extension. The determination of suitable efficiencies allows this method to be quantitative. (author) [pt

International comparison of methods to test the validity of dead-time and pile-up corrections for high-precision. gamma. -ray spectrometry

Energy Technology Data Exchange (ETDEWEB)

Houtermans, H.; Schaerf, K.; Reichel, F. (International Atomic Energy Agency, Vienna (Austria)); Debertin, K. (Physikalisch-Technische Bundesanstalt, Braunschweig (Germany, F.R.))

1983-02-01

The International Atomic Energy Agency organized an international comparison of methods applied in high-precision ..gamma..-ray spectrometry for the correction of dead-time and pile-up losses. Results of this comparison are reported and 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.)

Accurate determination and certification of bromine in plastic by isotope dilution inductively coupled plasma mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Ohata, Masaki, E-mail: m-oohata@aist.go.jp; Miura, Tsutomu

2014-07-21

Highlights: • Accurate analytical method of Br in plastic was studied by isotope dilution ICPMS. • A microwave acid digestion using quartz vessel was suitable for Br analysis. • Sample dilution by NH{sub 3} solution could remove memory effect for ICPMS measurement. • The analytical result of the ID-ICPMS showed consistency with that of INAA. • The ID-ICPMS developed could apply to certification of Br in candidate plastic CRM. - Abstract: The accurate analytical method of bromine (Br) in plastic was developed by an isotope dilution inductively coupled plasma mass spectrometry (ID-ICPMS). The figures of merit of microwave acid digestion procedures using polytetrafluoroethylene (PTFE) or quartz vessels were studied and the latter one was suitable for Br analysis since its material was free from Br contamination. The sample dilution procedures using Milli-Q water or ammonium (NH{sub 3}) solution were also studied to remove memory effect for ICPMS measurement. Although severe memory effect was observed on Milli-Q water dilution, NH{sub 3} solution could remove it successfully. The accuracy of the ID-ICPMS was validated by a certified reference material (CRM) as well as the comparison with the analytical result obtained by an instrumental neutron activation analysis (INAA) as different analytical method. From these results, the ID-ICPMS developed in the present study could be evaluated as accurate analytical method of Br in plastic materials and it could apply to certification of Br in candidate plastic CRM with respect to such regulations related to RoHS (restriction of the use of hazardous substances in electrical and electronics equipment) directive.

Fricke dosimetry: the difference between G(Fe3+) for 60Co gamma-rays and high-energy x-rays.

Science.gov (United States)

Klassen, N V; Shortt, K R; Seuntjens, J; Ross, C K

1999-07-01

A calibration of the Fricke dosimeter is a measurement of epsilon G(Fe3+). Although G(Fe3+) is expected to be approximately energy independent for all low-LET radiation, existing data are not adequate to rule out the possibility of changes of a few per cent with beam quality. When a high-precision Fricke dosimeter, which has been calibrated for one particular low-LET beam quality, is used to measure the absorbed dose for another low-LET beam quality, the accuracy of the absorbed dose measurement is limited by the uncertainty in the value of G(Fe3+). The ratio of G(Fe3+) for high-energy x-rays (20 and 30 MV) to G(Fe3+) for 60Co gamma-rays, G(Fe3+)MV(Co), was measured to be 1.007(+/-0.003) (confidence level of 68%) using two different types of water calorimeter, a stirred-water calorimeter (20 MV) and a sealed-water calorimeter (20, 30 MV). This value is consistent with our calculations based on the LET dependence of G(primary products) and, as well, with published measurements and theoretical treatments of G(Fe3+).

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.

Determination of fluorine concentrations using wavelength dispersive X-ray fluorescence (WDXRF) spectrometry to analyze fluoride precipitates.

Science.gov (United States)

Lee, H. A.; Lee, J.; Kwon, E.; Kim, D.; Yoon, H. O.

2015-12-01

In recent times, fluorine has been receiving increasing attention due to the possibility for chemical (HF) leakage accidents and its high toxicity to human and environment. In this respect, a novel approach for the determination of fluorine concentrations in water samples using wavelength dispersive X-ray fluorescence (WDXRF) spectrometry was investigated in this study. The main disadvantage of WDXRF technique for fluorine analysis is low analytical sensitivity for light elements with atomic number (Z) less than 15. To overcome this problem, we employed the precipitation reaction which fluoride is reacted with cation such as Al3+ and/or Ca2+ prior to WDXRF analysis because of their high analytical sensitivity. The cation was added in fluoride solutions to form precipitate (AlF3 and/or CaF2) and then the solution was filtered through Whatman filter. After drying at 60 °C for 5 min, the filter was coated with X-ray film and directly analyzed using WDXRF spectrometry. Consequently, we analyzed the cation on filter and subsequently fluorine concentration was calculated inversely based on chemical form of precipitate. This method can improve the analytical sensitivity of WDXRF technique for fluorine analysis and be applicable to various elements that can make precipitate.

Airborne gamma-ray spectrometry

DEFF Research Database (Denmark)

Hovgaard, Jens

A new method - Noise Adjusted Singular Value Decomposition, NASVD - for processing gamma-ray spectra has been developed as part of a Ph.D. project. By using this technique one is able to decompose a large set of data - for example from airborne gamma-ray surveys - into a few spectral components....... By knowing the spectral components and their amplitudes in each of the measured spectra one is able to extract more information from the data than possible with the methods used otherwise....

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.

Neutron activation analysis of lipsticks using gamma-ray spectrometry

International Nuclear Information System (INIS)

Mirsa, G.; Mittal, V.K.

2004-01-01

Neutron activation analysis with gamma-ray spectrometry was used to measure the concentrations of various elements in lipsticks of popular Indian and foreign brands. The aim of the present work was to study the possibility of existence of trace elements in samples of lipsticks (the ingredients of which are mostly organic in nature) and to see whether trace elements could distinguish lipsticks of different Indian and foreign brands from the forensic point of view apart from their inter-se differentiation. In the different samples of lipsticks that were analysed the following elements were detected: Au, Ba, Br, Ca, Cs, Fe, Na, Ru, Sb, Sc, Ta, Yb, Zn, Rb and Se. It was found that inter-se differentiation of lipsticks was possible on the basis of concentrations of trace elements and their profile. Concentration of bromine in samples of lipsticks identified lipsticks of different Indian brands. Samples of lipsticks of Indian and foreign brands could be differentiated on the basis of concentrations of cesium, antimony and scandium which were found to be higher in foreign brands as compared to those in Indian brands. (authors)

Self-absorption corrections of various sample-detector geometries in gamma-ray spectrometry using sample Monte Carlo Simulations

International Nuclear Information System (INIS)

Ahmad Saat; Appleby, P.G.; Nolan, P.J.

1997-01-01

Corrections for self-absorption in gamma-ray spectrometry have been developed using a simple Monte Carlo simulation technique. The simulation enables the calculation of gamma-ray path lengths in the sample which, using available data, can be used to calculate self-absorption correction factors. The simulation was carried out on three sample geometries: disk, Marinelli beaker, and cylinder (for well-type detectors). Mathematical models and experimental measurements are used to evaluate the simulations. A good agreement of within a few percents was observed. The simulation results are also in good agreement with those reported in the literature. The simulation code was carried out in FORTRAN 90,

Assessment of the suitability of different random number generators for Monte Carlo simulations in gamma-ray spectrometry

International Nuclear Information System (INIS)

Cornejo Diaz, N.; Vergara Gil, A.; Jurado Vargas, M.

2010-01-01

The Monte Carlo method has become a valuable numerical laboratory framework in which to simulate complex physical systems. It is based on the generation of pseudo-random number sequences by numerical algorithms called random generators. In this work we assessed the suitability of different well-known random number generators for the simulation of gamma-ray spectrometry systems during efficiency calibrations. The assessment was carried out in two stages. The generators considered (Delphi's linear congruential, mersenne twister, XorShift, multiplier with carry, universal virtual array, and non-periodic logistic map based generator) were first evaluated with different statistical empirical tests, including moments, correlations, uniformity, independence of terms and the DIEHARD battery of tests. In a second step, an application-specific test was conducted by implementing the generators in our Monte Carlo program DETEFF and comparing the results obtained with them. The calculations were performed with two different CPUs, for a typical HpGe detector and a water sample in Marinelli geometry, with gamma-rays between 59 and 1800 keV. For the Non-periodic Logistic Map based generator, dependence of the most significant bits was evident. This explains the bias, in excess of 5%, of the efficiency values obtained with this generator. The results of the application-specific assessment and the statistical performance of the other algorithms studied indicate their suitability for the Monte Carlo simulation of gamma-ray spectrometry systems for efficiency calculations.

Assessment of the suitability of different random number generators for Monte Carlo simulations in gamma-ray spectrometry.

Science.gov (United States)

Díaz, N Cornejo; Gil, A Vergara; Vargas, M Jurado

2010-03-01

The Monte Carlo method has become a valuable numerical laboratory framework in which to simulate complex physical systems. It is based on the generation of pseudo-random number sequences by numerical algorithms called random generators. In this work we assessed the suitability of different well-known random number generators for the simulation of gamma-ray spectrometry systems during efficiency calibrations. The assessment was carried out in two stages. The generators considered (Delphi's linear congruential, mersenne twister, XorShift, multiplier with carry, universal virtual array, and non-periodic logistic map based generator) were first evaluated with different statistical empirical tests, including moments, correlations, uniformity, independence of terms and the DIEHARD battery of tests. In a second step, an application-specific test was conducted by implementing the generators in our Monte Carlo program DETEFF and comparing the results obtained with them. The calculations were performed with two different CPUs, for a typical HpGe detector and a water sample in Marinelli geometry, with gamma-rays between 59 and 1800 keV. For the Non-periodic Logistic Map based generator, dependence of the most significant bits was evident. This explains the bias, in excess of 5%, of the efficiency values obtained with this generator. The results of the application-specific assessment and the statistical performance of the other algorithms studied indicate their suitability for the Monte Carlo simulation of gamma-ray spectrometry systems for efficiency calculations. Copyright 2009 Elsevier Ltd. All rights reserved.

Direct dating of Tantavel man by non-destructive gamma-ray spectrometry of fossil human skull Arago XXI

International Nuclear Information System (INIS)

Yokoyama, Yuji; Nguyen, Huu-Van

1981-01-01

A new method to date prehistoric samples is proposed. Non-destructive gamma-ray spectrometry with semi-conductor detector was used in the direct determination of the activities of 238 U, 234 U, 231 Pa, 230 Th and 228 Th. An age of (400sub(-96)sup(+infinite))x10 3 years was obtained from the 230 Th/ 238 U ratio of 0.975+-0.030 [fr

Accurate quasiparticle calculation of x-ray photoelectron spectra of solids.

Science.gov (United States)

Aoki, Tsubasa; Ohno, Kaoru

2018-05-31

It has been highly desired to provide an accurate and reliable method to calculate core electron binding energies (CEBEs) of crystals and to understand the final state screening effect on a core hole in high resolution x-ray photoelectron spectroscopy (XPS), because the ΔSCF method cannot be simply used for bulk systems. We propose to use the quasiparticle calculation based on many-body perturbation theory for this problem. In this study, CEBEs of band-gapped crystals, silicon, diamond, β-SiC, BN, and AlP, are investigated by means of the GW approximation (GWA) using the full ω integration and compared with the preexisting XPS data. The screening effect on a deep core hole is also investigated in detail by evaluating the relaxation energy (RE) from the core and valence contributions separately. Calculated results show that not only the valence electrons but also the core electrons have an important contribution to the RE, and the GWA have a tendency to underestimate CEBEs due to the excess RE. This underestimation can be improved by introducing the self-screening correction to the GWA. The resulting C1s, B1s, N1s, Si2p, and Al2p CEBEs are in excellent agreement with the experiments within 1 eV absolute error range. The present self-screening corrected GW approach has the capability to achieve the highly accurate prediction of CEBEs without any empirical parameter for band-gapped crystals, and provide a more reliable theoretical approach than the conventional ΔSCF-DFT method.

Accurate quasiparticle calculation of x-ray photoelectron spectra of solids

Science.gov (United States)

Aoki, Tsubasa; Ohno, Kaoru

2018-05-01

It has been highly desired to provide an accurate and reliable method to calculate core electron binding energies (CEBEs) of crystals and to understand the final state screening effect on a core hole in high resolution x-ray photoelectron spectroscopy (XPS), because the ΔSCF method cannot be simply used for bulk systems. We propose to use the quasiparticle calculation based on many-body perturbation theory for this problem. In this study, CEBEs of band-gapped crystals, silicon, diamond, β-SiC, BN, and AlP, are investigated by means of the GW approximation (GWA) using the full ω integration and compared with the preexisting XPS data. The screening effect on a deep core hole is also investigated in detail by evaluating the relaxation energy (RE) from the core and valence contributions separately. Calculated results show that not only the valence electrons but also the core electrons have an important contribution to the RE, and the GWA have a tendency to underestimate CEBEs due to the excess RE. This underestimation can be improved by introducing the self-screening correction to the GWA. The resulting C1s, B1s, N1s, Si2p, and Al2p CEBEs are in excellent agreement with the experiments within 1 eV absolute error range. The present self-screening corrected GW approach has the capability to achieve the highly accurate prediction of CEBEs without any empirical parameter for band-gapped crystals, and provide a more reliable theoretical approach than the conventional ΔSCF-DFT method.

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

International Nuclear Information System (INIS)

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

2004-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

Papadopoulou, D.N. [Laboratory of Analytical Chemistry, Faculty of Chemistry, Aristotle University, GR-54124, Thessaloniki (Greece); Zachariadis, G.A. [Laboratory of Analytical Chemistry, Faculty of Chemistry, Aristotle University, GR-54124, Thessaloniki (Greece); Anthemidis, A.N. [Laboratory of Analytical Chemistry, Faculty of Chemistry, Aristotle University, GR-54124, Thessaloniki (Greece); Tsirliganis, N.C. [Archaeometry Laboratory, Cultural and Educational Technology Institute, Tsimiski 58, GR-67100, Xanthi (Greece); Stratis, J.A. [Laboratory of Analytical Chemistry, Faculty of Chemistry, Aristotle University, GR-54124, Thessaloniki (Greece)]. E-mail: jstratis@chem.auth.gr

2004-12-01

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

Applications of gamma-ray spectrometry in real-time environmental monitoring

International Nuclear Information System (INIS)

Heath, R.L.; Dyer, N.C.

1974-01-01

The operation of large nuclear installations involves significant inventories of radioactive materials. Effective monitoring of effluent streams to permit evaluation of potential hazards which might result from discharge of radioisotopes is a requirement for safe operation of such facilities. The purpose of this paper is to present a summary of a program being conducted at the Idaho National Engineering Laboratory (INEL) to apply gamma-ray spectrometry to real-time isotopic monitoring of nuclear installations. The application of the lithium-drifted Ge spectrometer in the laboratory for isotopic assay is well established. To apply these techniques to routine on-line isotopic measurements requires the solution of a number of significant problems. These may be summarized as follows: the development of a remote pulse-height analyzer system; the development of adequate methods for analysis of pulse-amplitude spectra to permit isotopic assay and interpretation of results; and determination of basic nuclear decay data requirements for nuclides of interest to insure acceptance of isotopic assay results

Application of gamma ray spectrometry for evaluation of transfer factors in environmental matrices

International Nuclear Information System (INIS)

Rao, D.D.

2008-01-01

Gamma Ray Spectrometry (GRS) is performed using a variety of radiation detectors, to identify and determine radioactivity concentration of gamma emitting radionuclides qualitatively, in a wide range of samples. The samples can be of a high inventory power plant origin, NORM category or low level environmental samples, around a power plant. The method is usually applied to non-destructive analysis of environmental samples. However, it can also be applied to destructive analysis i.e. following extraction/separation of the analyte from the sample, if there is a need to pre-concentrate the analyte. The accuracy and precision of the method, depends on the quality of calibration, correction methods employed, stability of the system components, computational algorithms used, analysis of sources of uncertainties etc. The transfer factors among the environmental matrices are simple ratios, but the methodologies used in generating the respective concentrations have to be appropriately documented, including the validity of measurements. Validation mechanisms can include the results of international inter-comparison exercises, the certificates of standards issued by quality-accredited international laboratories. A few parameters involved in the qualitative analysis of gamma spectrometry are discussed here

Experimental observation of G banding verifying X-ray workers' chromosome translocation detected by FISH

International Nuclear Information System (INIS)

Sun Yuanming; Li Jin; Wang Qin; Tang Weisheng; Wang Zhiquan

2002-01-01

Objective: FISH is the most effective way of detecting chromosome aberration and many factors affect its accuracy. G-banding is used to verify the results of early X-ray workers' chromosome translocation examined by FISH. Methods: The chromosome translocations of early X-ray workers have been analysed by FISH (fluorescence in situ hybridization) and G-banding, yields of translocation treated with statistics. Results: The chromosome aberrations frequencies by tow methods are closely related. Conclusion: FISH is a feasible way to analyse chromosome aberrations of X-ray workers and reconstruct dose

Development of Wavelet Based Tools for Improving the γ-ray Spectrometry

International Nuclear Information System (INIS)

Hamzaoui, E-M.; El Badri, L.; Laraki, K.; Cherkaoui-Elmorsli, R.

2013-06-01

In this article, we propose a wavelet transform based tool to improve the use of gamma ray spectrometry as a nuclear technique. First, we attempt to study the problem of filtering the preamplifier's output signals of HPGe detector used in the measurements chain. Thus, we developed a nonlinear method based on discrete Coiflet transform combined to principal component analysis, which allows a significant improvement of the signal to noise ratio (SNR) at the output of the HPGe preamplifier. In a second step, the continuous wavelet transform, based on the Mexican Hat mother function, is used to achieve an automatic processing of the spectrometric data. This method permits us to get an alternative representation of the gamma energy spectrum. The results of different tests, performed in both the presence and the absence of a gamma radiation source, are illustrated. (authors)

Mass spectrometry

DEFF Research Database (Denmark)

Nyvang Hartmeyer, Gitte; Jensen, Anne Kvistholm; Böcher, Sidsel

2010-01-01

Matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF MS) is currently being introduced for the rapid and accurate identification of bacteria. We describe 2 MALDI-TOF MS identification cases - 1 directly on spinal fluid and 1 on grown bacteria. Rapidly obtained...

SEARCHING FOR OVERIONIZED PLASMA IN THE GAMMA-RAY-EMITTING SUPERNOVA REMNANT G349.7+0.2

Energy Technology Data Exchange (ETDEWEB)

Ergin, T.; Sezer, A. [TUBITAK Space Technologies Research Institute, ODTU Campus, 06531, Ankara (Turkey); Saha, L.; Majumdar, P. [Saha Institute of Nuclear Physics, Kolkata, West Bengal 700064 (India); Gök, F. [Akdeniz University, Faculty of Education, Department of Secondary Science and Mathematics Education, Antalya, 07058 (Turkey); Ercan, E. N., E-mail: tulun.ergin@tubitak.gov.tr [Bogazici University, Physics Department, Bebek, 34342, Istanbul (Turkey)

2015-05-10

G349.7+0.2 is a supernova remnant (SNR) expanding in a dense medium of molecular clouds and interacting with clumps of molecular material emitting gamma-rays. We analyzed the gamma-ray data of the Large Area Telescope on board the Fermi Gamma-Ray Space Telescope and detected G349.7+0.2 in the energy range of 0.2–300 GeV with a significance of ∼13σ, showing no extended morphology. Modeling of the gamma-ray spectrum revealed that the GeV gamma-ray emission dominantly originates from the decay of neutral pions, where the protons follow a broken power-law distribution with a spectral break at ∼12 GeV. To search for features of radiative recombination continua in the eastern and western regions of the remnant, we analyzed the Suzaku data of G349.7+0.2 and found no evidence for overionized plasma. In this paper, we discuss possible scenarios to explain the hadronic gamma-ray emission in G349.7+0.2 and the mixed morphology nature of this SNR.

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)

Chemical preparation of biological materials for accurate chromium determination by isotope dilution mass spectrometry

International Nuclear Information System (INIS)

Dunstan, L.P.; Garner, E.L.

1977-01-01

The current interest in trace elements in biological materials has created a need for accurate methods of analysis. The source of discrepancies and variations in chromium concentration determinations is often traceable to inadequate methods of sample preparation. Any method of Cr analysis that requires acid digestion of a biological matrix must take into consideration the existence or formation of a volatile Cr component. In addition, because Cr is often present at concentrations less than 1 μg/g, the analytical blank becomes a potential source of error. Chemical procedures have been developed for the digestion of the biological matrix and the separation of Cr without either large analytical blanks or significant losses by volatilization. These procedures have been used for the analysis of NBS Standard Reference Material (SRM) 1569 Brewers Yeast; SRM 1577 Bovine Liver; SRM 1570 Spinach and other biological materials including human hair and nails. At this time, samples containing 1 μg of Cr can be determined with an estimated accuracy of 2 percent

Prompt gamma-ray spectrometry for measurement of B-10 concentration in brain tissue and blood

International Nuclear Information System (INIS)

Nakagawa, Yoshinobu; Kitamura, Katsuji; Kobayashi, Toru; Matsumoto, Keizo; Hatanaka, Hiroshi.

1993-01-01

Boron-10 (B-10) concentration in the brain tissue and blood was measured continuously for 24 hours after injection of the B-10 compound in live rabbits using prompt gamma-ray spectrometry. Following injection of B-10 compound (Na 2 B 12 H 11 SH, 50mg/kg) dissolved in physiological saline, B-10 concentration was continuously measured in the brain tissue. Intermittently the concentration of B-10 in blood and cerebro-spinal fluid (CSF) was also measured. In 10 minutes after the injection of B-10 compound, the level of B-10 concentration reached the peak of 400-500 ppm in blood and 20-30 ppm in the normal brain tissue. In 60 minutes the level of B-10 concentration rapidly decreased and then a gradual decline was observed. The value was 15-30 ppm at 3 hours after injection, 5-10 ppm at 6 hours and 2-5 ppm at 24 hours in the blood. The concentration in the brain tissue was 3-8 ppm at 3 hours, 2-5 ppm at 6 hours and below 1.5 ppm at 24 hours. B-10 concentration in cerebro-spinal fluid was below 1 ppm. B-10 concentration was also measured in the brain tumor and blood in the human cases at boron neutron capture therapy (BNCT). These data studied by prompt gamma-ray spectrometry are very important and useful to decide the irradiation time. (author)

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

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)

Ways for accurate analysis of high purity materials using the glow discharge mass spectrometry (GD-MS); Wege zur genauen Charakterisierung hochreiner Materialien mit der Glimmentladungs-Massenspektrometrie (GD-MS)

Energy Technology Data Exchange (ETDEWEB)

Gusarova, Tamara

2010-04-14

The main aim of this work consists in the investigation, development and application of improved possibilities of accurate analysis of high purity materials using the solid sample technique of Glow Discharge Mass Spectrometry (GD-MS), as well as in the sensitivity enhancement of GD Optical Emission Spectrometry (GD-OES) by implicating the hollow cathode effect. The emphasis of the PhD thesis consists in the accurate quantification for GD-MS. As appropriate certified reference materials (CRMs) for calibration are lacking in most cases an accurate quantification especially for trace elements mass fractions at {mu}g kg{sup -1} level can often not be achieved. To overcome this problem and to expand the possibilities of modern GD-MS hereby, synthetic standards were applied for calibration of both high resolution GD-MS instruments ''VG 9000'' and ''Element GD''. The standards were prepared by doping of matrix powder with trace element standard solutions followed by drying and pressing the doped powder to compact pellets. With the quantification approach worked out and described here accurate analysis results with small uncertainties can be achieved for most elements of periodic table in almost every matrix composition. Furthermore direct traceability of the analytical results to the International System of Units (SI) is provided ensuring their higher metrological quality. Numerous additional systematic investigations concerning the preparation of the synthetic standards and their properties were carried out. The results of calibration of GD-MS instruments with synthetic standards for Co (Co-C), Cu, In, Fe and Zn matrices were checked by measuring CRMs. These results were also contrasted with those of other quantification approaches, as usually used in GD-MS routine. The results achieved with synthetic standards had the highest accuracy. The successful participation in the round robin test CCQM-P107 between international

European coordination of environmental airborne gamma ray spectrometry. Final report 1999

International Nuclear Information System (INIS)

Sanderson, D.C.; McLeod, J.J.

1999-04-01

This Concerted Action was funded under the EURATOM Nuclear Fission Safety Programme of the Fourth Framework Programme, and was initiated to address transnational issues relating to environmental airborne gamma ray spectrometry (AGS). Significant development of AGS systems and teams has taken place within Europe during the period following the Chernobyl accident. The technique is increasingly recognised as particularly relevant to emergency response. It is also uniquely capable of acquiring data on anthropogenic and natural radionuclides on regional, national and international scales, for reference purposes, ecological studies and epidemiological research. Prior to this EU programme the methodologies and systems used by European AGS teams had undergone rapid and largely uncoordinated development. This raised questions about comparability of systems, applications, and data between teams, duplication of research, the scope for transnational cooperation and standardisation, and future research and development needs in the field. This project, which brought together ten AGS teams from across Europe, was formed to address these issues. The work was conducted in three stages and has largely succeeded in its objectives. An active communication network was developed for collaboration and exchange of information, and to start the process of harmonisation of the different methodologies used by individual AGS teams. Two formal partners' meetings were organised, the first aimed at defining the EU capability in AGS, the second, in the form of an international symposium (RADMAGS), was aimed at reviewing developments on future research needs and the scope for standardisation. This report gives full details of the project and its deliverables together with discussion of the further needs in support of transnational harmonisation of this topic. The European Capability for AGS was defined at an early stage of the project, and monitored throughout. An EU Bibliography on AGS

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)

Developments in gamma-ray spectrometry: systems, software, and methods-II. 3. Low-Energy Gamma-Ray Spectrometry Using a Compton-Suppressed Telescope Detector

International Nuclear Information System (INIS)

Sigg, R.A.; DiPrete, D.P.

2001-01-01

The Savannah River Technology Center (SRTC) utilizes gamma-ray spectrometry in studying numerous areas of applied interest to the Savannah River Site (SRS). For example, analyses of long-lived gamma-ray-emitting fission products and actinides are required to meet waste characterization, process holdup, environmental restoration, and decontamination and decommissioning efforts. A significant portion of the overall effort centers on measurements of gamma rays having energies below several hundred kilo-electron-volts. To assist these efforts, the SRTC recently acquired a spectrometer system that provides lower natural and Compton scattered background levels while achieving relatively high counting efficiencies for low-energy gamma rays. The combination of high efficiency and low background provides factor-of- 2-to-4 improvements in minimum detectable activities and allows meeting programmatic objectives with shorter measurement times. Numerous Compton-suppression spectrometers have been reported since the concept was first advanced. The spectrometer consists of two high-purity germanium detectors in a telescope configuration surrounded by a background /Compton-suppression sodium iodide detector. The front germanium detector is a 20-mm-thick x 60-mm-diam broad energy spectrometer, and the rear detector is a 40% efficient 61- mm-diam x 60-cm-thick closed-end coaxial spectrometer. The cryostat housing the germanium detectors (a) includes a carbon composite window for transmitting low-energy gamma rays, (b) is in a J-type configuration to mask the germanium detectors from natural activities in the cryo-pumping media, and (c) is fabricated from materials selected for low background. The telescope detector is in the 8.6-cm-inside-diameter annulus of a 22.9- x 22.9-cm sodium iodide detector encased in a 10-cm-thick lead shield. The counting system is located in a basement counting room having ∼60-cm-thick concrete walls. Initial tests show that the low-energy segment of

Simulation of the isotopic ratio determination of plutonium by Ge(Li) gamma-ray spectrometry

International Nuclear Information System (INIS)

Baba, Hiroshi; Yagi, Hideyuki

1979-09-01

A simulation program ''SIMPUG'' was developed for assessing feasibility of the isotopic ratio determination of plutonium by Ge(Li) γ-ray spectrometry. The program consists of (1) construction of the spectrum profiles for eight peak groupings of interest with a given set of isotopic compositions and by the use of the known nuclear data for emitting γ rays and (2) determination of the intensity of each participating nuclide following a presently developed algorithm of spectrum unfolding. Effects of various factors on the reliability of the results were examined with the simulation program. Accuracy of the results was found to be little affected by the change of the detector resolution if the spectrum was taken with sufficient expansion. Counting statistics was concluded to be the most essential factor for the precision of the results, while the aging effect was not found significant. Contamination of fission products beyond a certain level brought about fatal errors in the determined values, particularly in the case of minor components. (author)

Neutron activation analysis of ultrabasis rock by Ge(Li) γ-ray spectrometry and group separation

International Nuclear Information System (INIS)

Chen Baoguan; Yuan Ling; Fang Chanmeng

1986-01-01

The analytical procedure for determination of 21 elements in two ultrabasis rock samples with Ge(Li) gamma-ray spectrometry and group separation was described. 8 elements including Cr, Fe, Co, Sc, Mn, Na, Cl and Br have been directly determined by INAA. 13 elements including La, Ce, Nd, Sm, Gd, Eu, Tb, Ho, Tm, Yb, Lu, Zn and Cs have been determined by radiochemical separation. The samples of international standard AGV-1 (Andesite) have also been analyzed. The agreement of the results with the values proposed by F.J.Flanagan is satisfactory

A New Method for Processing Airborne Gamma Ray Spectrometry Data for Mapping Low Level Contaminations

DEFF Research Database (Denmark)

Aage, Helle Karina; Korsbech, Uffe C C; Bargholz, Kim

1999-01-01

A new technique for processing airborne gamma ray spectrometry data has been developed. It is based on the noise adjusted singular value decomposition method introduced by Hovgaard in 1997. The new technique opens for mapping of very low contamination levels. It is tested with data from Latvia...... where the remaining contamination from the 1986 Chernobyl accident together with fallout from the atmospheric nuclear weapon tests includes Cs-137 at levels often well below 1 kBq/m(2) equivalent surface contamination. The limiting factors for obtaining reliable results are radon in the air, spectrum...

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

Development of isotope dilution-liquid chromatography/mass spectrometry combined with standard addition techniques for the accurate determination of tocopherols in infant formula

Energy Technology Data Exchange (ETDEWEB)

Lee, Joonhee; Jang, Eun-Sil; Kim, Byungjoo, E-mail: byungjoo@kriss.re.kr

2013-07-17

Graphical abstract: -- Highlights: •ID-LC/MS method showed biased results for tocopherols analysis in infant formula. •H/D exchange of deuterated tocopherols in sample preparation was the source of bias. •Standard addition (SA)-ID-LC/MS was developed as an alternative to ID-LC/MS. •Details of calculation and uncertainty evaluation of the SA-IDMS were described. •SA-ID-LC/MS showed a higher-order metrological quality as a reference method. -- Abstract: During the development of isotope dilution-liquid chromatography/mass spectrometry (ID-LC/MS) for tocopherol analysis in infant formula, biased measurement results were observed when deuterium-labeled tocopherols were used as internal standards. It turned out that the biases came from intermolecular H/D exchange and intramolecular H/D scrambling of internal standards in sample preparation processes. Degrees of H/D exchange and scrambling showed considerable dependence on sample matrix. Standard addition-isotope dilution mass spectrometry (SA-IDMS) based on LC/MS was developed in this study to overcome the shortcomings of using deuterium-labeled internal standards while the inherent advantage of isotope dilution techniques is utilized for the accurate recovery correction in sample preparation processes. Details of experimental scheme, calculation equation, and uncertainty evaluation scheme are described in this article. The proposed SA-IDMS method was applied to several infant formula samples to test its validity. The method was proven to have a higher-order metrological quality with providing very accurate and precise measurement results.

The participation of ATOMKI in the G-2 international intercomparison of high precision gamma-ray spectrometry measurements

International Nuclear Information System (INIS)

Gaspar, A.; Lakatos, T.; Sulik, B.; Toeroek, I.

1981-01-01

International intercomparison had been organized by the IAEA in high precision gamma spectrometry. Five mixed-spectrum sources were prepared and sent to the participants by the IAEA for relative gamma emission rate measurements. This source type enables the whole measuring method and procedure to be tested. Measurements were carried out using two independent methods: a.) simple normalization to an additional radioactive source; b.) using a time variant pulse processor and random pulse generator for correction of dead-time and pile-up losses. The results agreed in most cases within +-1% with the IAEA results. (R.J.)

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)

Gamma-ray spectrometry data collection and reduction by simple computing systems

International Nuclear Information System (INIS)

Op de Beeck, J.

1975-01-01

The review summarizes the present state of the involvement of relatively small computing devices in the collection and processing of gamma-ray spectrum data. An economic and utilitarian point of view has been chosen with regard to data collection in order to arrive at practically valuable conclusions in terms of feasibility of possible configurations with respect to their eventual application. A unified point of view has been adopted with regard to data processing by developing an information theoretical approach on a more or less intuitive level in an attempt to remove the largest part of the virtual disparity between the several processing methods described in the literature. A synoptical introduction to the most important mathematical methods has been incorporated, together with a detailed theoretical description of the concept gamma-ray spectrum. In accordance with modern requirements, the discussions are mainly oriented towards high-resolution semiconductor detector-type spectra. The critical evaluation of the processing methods reviewed is done with respect to a set of predefined criteria. Smoothing, peak detection, peak intensity determination, overlapping peak resolving and detection and upper limits are discussed in great detail. A preferred spectrum analysis method combining powerful data reduction properties with extreme simplicity and speed of operation is suggested. The general discussion is heavily oriented towards activation analysis application, but other disciplines making use of gamma-ray spectrometry will find the material presented equally useful. Final conclusions are given pointing to future developments and shifting their centre of gravity towards improving the quality of the measurements rather than expanding the use of tedious and sophisticated mathematical techniques requiring the limits of available computational power. (author)

Radon fixation for determination of 224Ra, 226Ra and 228Ra via gamma-ray spectrometry

International Nuclear Information System (INIS)

Herranz, M.; Idoeta, R.; Abelairas, A.; Legarda, F.

2006-01-01

The aim of this work is the improvement of the procedure for the determination of radium isotopes activities in water, which is done through radiochemical separation and subsequent gamma-ray spectrometry. In addition, radon gas retention is studied using different activated carbon materials. The results of the IAEA Proficiency test: 'Determination of radium and uranium radionuclides in water' of December 2002 [IAEA, 2003. Analytical quality control services: determination of radium and uranium radionuclides in water. Preliminary Report, Seibersdorf] are considered for this work

Direct determination of trace elements in boron nitride powders by slurry sampling total reflection X-ray fluorescence spectrometry

Energy Technology Data Exchange (ETDEWEB)

Amberger, Martin A.; Hoeltig, Michael [University of Hamburg, Institute for Inorganic and Applied Chemistry, Martin-Luther-King-Platz 6, D-20146 Hamburg (Germany); Broekaert, Jose A.C., E-mail: jose.broekaert@chemie.uni-hamburg.d [University of Hamburg, Institute for Inorganic and Applied Chemistry, Martin-Luther-King-Platz 6, D-20146 Hamburg (Germany)

2010-02-15

The use of slurry sampling total reflection X-ray fluorescence spectrometry (SlS-TXRF) for the direct determination of Ca, Cr, Cu, Fe, Mn and Ti in four boron nitride powders has been described. Measurements of the zeta potential showed that slurries with good stabilities can be obtained by the addition of polyethylenimine (PEI) at a concentration of 0.1 wt.% and by adjusting the pH at 4. For the optimization of the concentration of boron nitride in the slurries the net line intensities and the signal to background ratios were determined for the trace elements Ca and Ti as well as for the internal standard element Ga in the case of concentrations of boron nitride ranging from 1 to 30 mg mL{sup -1}. As a compromise with respect to high net line intensities and high signal to background ratios, concentrations of 5 mg mL{sup -1} of boron nitride were found suitable and were used for all further measurements. The limits of detection of SlS-TXRF for the boron nitride powders were found to range from 0.062 to 1.6 mug g{sup -1} for Cu and Ca, respectively. Herewith, they are higher than those obtained in solid sampling and slurry sampling graphite furnace atomic absorption spectrometry (SoS-GFAAS, SlS-GFAAS) as well as those of solid sampling electrothermal evaporation inductively coupled plasma optical emission spectrometry (SoS-ETV-ICP-OES). For Ca and Fe as well as for Cu and Fe, however, they were found to be lower than for GFAAS and for ICP-OES subsequent to wet chemical digestion, respectively. The universal applicability of SlS-TXRF to the analysis of samples with a wide variety of matrices could be demonstrated by the analysis of certified reference materials such as SiC, Al{sub 2}O{sub 3}, powdered bovine liver and borate ore with a single calibration. The correlation coefficients of the plots for the values found for Ca, Fe and Ti by SlS-TXRF in the boron nitride powders as well as in the before mentioned samples versus the reference values for the respective

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...

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)

Accurate determination of selected pesticides in soya beans by liquid chromatography coupled to isotope dilution mass spectrometry.

Science.gov (United States)

Huertas Pérez, J F; Sejerøe-Olsen, B; Fernández Alba, A R; Schimmel, H; Dabrio, M

2015-05-01

A sensitive, accurate and simple liquid chromatography coupled with mass spectrometry method for the determination of 10 selected pesticides in soya beans has been developed and validated. The method is intended for use during the characterization of selected pesticides in a reference material. In this process, high accuracy and appropriate uncertainty levels associated to the analytical measurements are of utmost importance. The analytical procedure is based on sample extraction by the use of a modified QuEChERS (quick, easy, cheap, effective, rugged, safe) extraction and subsequent clean-up of the extract with C18, PSA and Florisil. Analytes were separated on a C18 column using gradient elution with water-methanol/2.5 mM ammonium acetate mobile phase, and finally identified and quantified by triple quadrupole mass spectrometry in the multiple reaction monitoring mode (MRM). Reliable and accurate quantification of the analytes was achieved by means of stable isotope-labelled analogues employed as internal standards (IS) and calibration with pure substance solutions containing both, the isotopically labelled and native compounds. Exceptions were made for thiodicarb and malaoxon where the isotopically labelled congeners were not commercially available at the time of analysis. For the quantification of those compounds methomyl-(13)C2(15)N and malathion-D10 were used respectively. The method was validated according to the general principles covered by DG SANCO guidelines. However, validation criteria were set more stringently. Mean recoveries were in the range of 86-103% with RSDs lower than 8.1%. Repeatability and intermediate precision were in the range of 3.9-7.6% and 1.9-8.7% respectively. LODs were theoretically estimated and experimentally confirmed to be in the range 0.001-0.005 mg kg(-1) in the matrix, while LOQs established as the lowest spiking mass fractionation level were in the range 0.01-0.05 mg kg(-1). The method reliably identifies and quantifies the

Design and construction of the gamma ray transmission tomographer g-TAC-02

International Nuclear Information System (INIS)

Pavon Hernandez, Noriel; Ravelo Sanchez, Alberto; Idel, Pedro; Macias Perez, Rafael; Garcia Trapaga, Cesar; Campos Montenegro, Augusto

2000-01-01

An equipment for gamma ray transmission tomographer was designed and constructed in the Higher Institute of Nuclear Sciences and Technology. It was the g-TAC-01, based on a nuclear instrumentation, a mechanic instrumentation, and the control of the system from a personal computer. This first version permitted to obtain the know how of the technology of construction of equipment for tomography. The present work describes the second version of the gamma ray transmission tomographer: the g-TAC-02, with very important upgrading in the control session. Now the control system is a microcontroller based, electronic control system, designed to work in multiples forms: manual, automatic and with the computer

Highly accurate determination of relative gamma-ray detection efficiency for Ge detector and its application

International Nuclear Information System (INIS)

Miyahara, H.; Mori, C.; Fleming, R.F.; Dewaraja, Y.K.

1997-01-01

When quantitative measurements of γ-rays using High-Purity Ge (HPGe) detectors are made for a variety of applications, accurate knowledge of oy-ray detection efficiency is required. The emission rates of γ-rays from sources can be determined quickly in the case that the absolute peak efficiency is calibrated. On the other hand, the relative peak efficiencies can be used for determination of intensity ratios for plural samples and for comparison to the standard source. Thus, both absolute and relative detection efficiencies are important in use of γ-ray detector. The objective of this work is to determine the relative gamma-ray peak detection efficiency for an HPGe detector with the uncertainty approaching 0.1% . We used some nuclides which emit at least two gamma-rays with energies from 700 to 2400 keV for which the relative emission probabilities are known with uncertainties much smaller than 0.1%. The relative peak detection efficiencies were calculated from the measurements of the nuclides, 46 Sc, 48 Sc, 60 Co and 94 Nb, emitting two γ- rays with the emission probabilities of almost unity. It is important that various corrections for the emission probabilities, the cascade summing effect, and the self-absorption are small. A third order polynomial function on both logarithmic scales of energy and efficiency was fitted to the data, and the peak efficiency predicted at certain energy from covariance matrix showed the uncertainty less than 0.5% except for near 700 keV. As an application, the emission probabilities of the 1037.5 and 1212.9 keV γ-rays for 48 Sc were determined using the function of the highly precise relative peak efficiency. Those were 0.9777+0,.00079 and 0.02345+0.00017 for the 1037.5 and 1212.9 keV γ-rays, respectively. The sum of these probabilities is close to unity within the uncertainty which means that the certainties of the results are high and the accuracy has been improved considerably

A comparative study for the correction of random gamma ray summing effect in HPGe - detector based gamma ray spectrometry

International Nuclear Information System (INIS)

Rajput, M.U.

2007-01-01

Random coincidence summing of gamma rays is a potential source of errors in gamma ray spectrometry. The effect has a little significance at low counting rates but becomes increasingly important at high counting rates. Careful corrections are required to avoid the introduction of errors in quantitative based measurements. Several correction methods have been proposed. The most common is the pulser method that requires a precision Pulse Generator in the electronic circuitry to provide reference peak. In this work, a comparative study has been carried out both by using pulser method and utilizing radioactive source based method. This study makes the use of 137 Cs radionuclide as a fixed source and the 241 Am as a varied source. The dead time of the system has been varied and the acquisition of the spectra at each position yielded the resulted peak areas with pulsed pile up losses. The linear regression of the data has been carried out. The study has resulted in establishing a consistent factor that can be used as the characteristic of the detector and thereby removes the need of the calibrated or precise Pulse Generator. (author)

A low-energy set-up for gamma-ray spectrometry of NORM tailored to the needs of a secondary smelting facility.

Science.gov (United States)

Lutter, G; Schreurs, I Vandael; Croymans, T; Schroeyers, W; Schreurs, S; Hult, M; Marissens, G; Stroh, H; Tzika, F

2017-08-01

A measurement station dedicated for quantitative radiological characterisation of naturally occurring radionuclides in a metallurgical company and based on gamma-ray spectrometry was developed. The station is intended for performing quality control of final non-ferrous metal products and for radiological checks of incoming materials. A low-background point-contact HPGe-detector was used and the signal was split in two branches to enable collecting simultaneously spectra with high amplification (for gamma-ray energies below 250keV) and low amplification. Copyright © 2017 The Authors. Published by Elsevier Ltd.. All rights reserved.

Crystallization and preliminary X-ray analysis of Chandipura virus glycoprotein G

International Nuclear Information System (INIS)

Baquero, Eduard; Buonocore, Linda; Rose, John K.; Bressanelli, Stéphane; Gaudin, Yves; Albertini, Aurélie A.

2012-01-01

Chandipura virus glycoprotein ectodomain (Gth) was purified and crystallized at pH 7.5. X-ray diffraction data set was collected to a resolution of 3.1 Å. Fusion in members of the Rhabdoviridae virus family is mediated by the G glycoprotein. At low pH, the G glycoprotein catalyzes fusion between viral and endosomal membranes by undergoing a major conformational change from a pre-fusion trimer to a post-fusion trimer. The structure of the G glycoprotein from vesicular stomatitis virus (VSV G), the prototype of Vesiculovirus, has recently been solved in its trimeric pre-fusion and post-fusion conformations; however, little is known about the structural details of the transition. In this work, a soluble form of the ectodomain of Chandipura virus G glycoprotein (CHAV G th ) was purified using limited proteolysis of purified virus; this soluble ectodomain was also crystallized. This protein shares 41% amino-acid identity with VSV G and thus its structure could provide further clues about the structural transition of rhabdoviral glycoproteins induced by low pH. Crystals of CHAV G th obtained at pH 7.5 diffracted X-rays to 3.1 Å resolution. These crystals belonged to the orthorhombic space group P2 1 2 1 2, with unit-cell parameters a = 150.3, b = 228.2, c = 78.8 Å. Preliminary analysis of the data based on the space group and the self-rotation function indicated that there was no trimeric association of the protomers. This unusual oligomeric status could result from the presence of fusion intermediates in the crystal

Accurate argon cluster-ion sputter yields: Measured yields and effect of the sputter threshold in practical depth-profiling by x-ray photoelectron spectroscopy and secondary ion mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Cumpson, Peter J.; Portoles, Jose F.; Barlow, Anders J.; Sano, Naoko [National EPSRC XPS User' s Service (NEXUS), School of Mechanical and Systems Engineering, Newcastle University, Newcastle upon Tyne, NE1 7RU (United Kingdom)

2013-09-28

Argon Gas Cluster-Ion Beam sources are likely to become widely used on x-ray photoelectron spectroscopy and secondary ion mass spectrometry instruments in the next few years. At typical energies used for sputter depth profiling the average argon atom in the cluster has a kinetic energy comparable with the sputter threshold, meaning that for the first time in practical surface analysis a quantitative model of sputter yields near threshold is needed. We develop a simple equation based on a very simple model. Though greatly simplified it is likely to have realistic limiting behaviour and can be made useful for estimating sputter yields by fitting its three parameters to experimental data. We measure argon cluster-ion sputter yield using a quartz crystal microbalance close to the sputter threshold, for silicon dioxide, poly(methyl methacrylate), and polystyrene and (along with data for gold from the existing literature) perform least-squares fits of our new sputter yield equation to this data. The equation performs well, with smaller residuals than for earlier empirical models, but more importantly it is very easy to use in the design and quantification of sputter depth-profiling experiments.

Correcting the effects of the matrix using capture gamma-ray spectrometry: Application to measurement by Active Neutron Interrogation; Correction des effets de matrice par spectrometrie des rayonnements gamma de capture: Application a la mesure par Interrogation Neutronique Active (I.N.A.)

Energy Technology Data Exchange (ETDEWEB)

Baudry, G.

2003-11-15

In the field of the measurement of low masses of fissile material ({sup 235}U, {sup 239}Pu, {sup 241}Pu) in radioactive waste drums, the Active Neutron Interrogation is a non-destructive method achieving good results. It does however remain reliant upon uncertainties related to the matrix effects on interrogation and fission neutrons. The aim of this thesis is to develop a correction method able to take into account these matrix effects by quantifying the amount of absorbent materials (chlorine and hydrogen) in a 118- liter homogeneous matrix. The main idea is to use the gamma-ray spectrometry of gamma emitted by neutron captures to identify and quantify the composition of the matrix. An indicator from its chlorine content is then deduced in order to choose the calibration coefficient which best represents the real composition of the matrix. This document firstly presents the needs of control and characterization of radioactive objects, and the means used in the field of nuclear measurement. Emphases is put in particular on the Active Neutron Interrogation method. The matrices of interest are those made of light technological waste (density {<=} 0,4 g/cm{sup 3}) containing hydrogenated and chlorinated materials. The advantages of gamma-rays emitted by neutron captures for the determination of a chlorine content indicator of the matrices and the principles of the correction method are then explained. Measurements have been firstly realized with an existing Neutron Interrogation device (PROMETHEE 6). Such measurements have proven its inadequacy: no signal from the matrix hydrogen was detected, due to an intense signal from the polyethylene contained in some cell elements. Moreover, the matrix chlorine content appeared difficult to be measured. A new and specific device, named REGAIN and dedicated to active gamma-rays spectrometry, was defined with the Monte-Carlo N-Particle (MCNP) code. The experiments conducted with this new device made it possible to detect the

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

Improvements in Applied Gamma-Ray Spectrometry with Germanium Semiconductor Detector

Energy Technology Data Exchange (ETDEWEB)

Brune, D; Hellstroem, S [AB Atomenergi, Nykoeping (Sweden); Dubois, J [Chalmers University of Technology, Goeteborg (Sweden)

1965-01-15

A germanium semi-conductor detector has in the present investigation been used in four cases of applied gamma-ray spectrometry. In one case the weak-activity contribution of Cs{sup 134} in Cs{sup 137} standard sources has been determined. The second case concerns the determination of K{sup 42} in samples of biological origin containing strong Na{sup 24} activities. In the third case the Nb{sup 94} and Nb{sup 95} activities from neutron-irradiated niobium foils used in the dosimetry of high neutron fluxes with long exposure times have been completely resolved and it has been possible to determine the ratio of the two activities with a high degree of accuracy. Finally, a Zr{sup 95} - Nb{sup 95} source has been analysed in a similar way with respect to its radiochemical composition. The resolution obtained also made possible a determination of the branching ratio of the two gamma-transitions in Zr{sup 95} and of the energies of the gamma-transitions of both nuclides.

Use of airborne gamma-ray spectrometry for kaolin exploration

Science.gov (United States)

Tourlière, B.; Perrin, J.; Le Berre, P.; Pasquet, J. F.

2003-08-01

Airborne gamma-ray spectrometry was used to define targets with kaolin potential in the Armorican Massif of Brittany, France. This exploration method is based on the principle that kaolinite, an aluminosilicate clay mineral constituting kaolin, is formed by the hydrolysis of potash feldspar with the elimination of potassium. Therefore, potassium contrast between favourable host-rock such as a leucogranite and kaolin occurrence is likely a significant pathfinder. As the relationship between the potassium-40 recorded by an airborne gamma-ray spectrometer and total potassium is constant, such data provide us a direct measurement of the potassium content of the ground flown over. Our study tested this by calculating, for each geological unit, the difference between the measured and average potassium content calculated for a given geological formation. The study was based on (i) a recent (1998) high-definition airborne geophysical survey over the Armorican Massif undertaken on behalf of the French Government, and (ii) new geological compilation maps covering the same region. Depleted zones, where the measured potassium is less than the average potassium content calculated target areas with high potential of containing kaolin, provided that the unit was originally rich in potash feldspar. By applying this method to the entire Armorican Massif, it was possible to identify 150 potassium-depleted zones, including 115 that were subjected to rapid field checks and 36 that contained kaolin (21 new discoveries). This method, which is both safe for the environment and easy to use, is therefore a good tool for rapidly defining targets with kaolin potential at a regional scale. The method may also have possibilities in exploring for other types of deposit characterised by an enrichment or depletion in U, K and/or Th.

KD901G X-ray system to reject contaminants

International Nuclear Information System (INIS)

Shinohara, Hachiro

1995-01-01

Among the complaints to the foods that consumers bought, the proportion of the mixing of alien substances is more than 20%. The number of the cases classified by the kinds of alien substances, and that of minerals and animal substances are shown. The causes of the mixing of alien substances are classified into those due to the mixing in raw materials, production places, processing machines and workers. In case of using primary products as raw materials, the alien substances closely related to those raw materials are difficult to detect, such as bones and hairs in animal meat, fish bones, egg shells and fruit seeds. There are problems and limitation in the inspection of alien substance mixing by visual or touching inspection, metal detectors and the visual inspection of X-ray radiographs. The judgement of the presence of alien substances by automatically processing X-ray radiograph information has been tried one or two-dimensionally. The X-ray alien substance detector KD901G adopted the one-dimensional line sensor type, and its features are shown. The effective introduction of the X-ray alien substance detector, its comparison with metal detectors, and the safety of workers against radiation exposure and the safety of inspected foods are discussed. (K.I.)

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.)

Chemical analysis of refractories by plasma spectrometry

International Nuclear Information System (INIS)

Coutinho, C.A.

1990-01-01

X-ray spectrometry has been, since the last two or three decades, the traditional procedure for the chemical analysis of refractories, due to its high degree of accuracy and speed to produce analytical results. An interesting alternative to X-ray fluorescence is provided by the Inductively Coupled Plasma Spectrometry technique, for those laboratories where wet chemistry facilities are already available or process control is not required at high speed, or investiment costs have to be low. This paper presents results obtained by plasma spectroscopy for the analysis of silico - aluminous refractories, showing calibration curves, precion and detection limits. Considerations and comparisons with X-ray fluorescence are also made. (author) [pt

Accurate determination of 129I concentrations and 129I/137Cs ratios in spent nuclear resins by Accelerator Mass Spectrometry

International Nuclear Information System (INIS)

Nottoli, Emmanuelle; Bienvenu, Philippe; Labet, Alexandre; Bourlès, Didier; Arnold, Maurice; Bertaux, Maité

2014-01-01

Determining long-lived radionuclide concentrations in radioactive waste has fundamental implications for the long-term management of storage sites. This paper focuses on the measurement of low 129 I contents in ion exchange resins used for primary fluid purification in Pressurised Water Reactors (PWR). Iodine-129 concentrations were successfully determined using Accelerator Mass Spectrometry (AMS) following a chemical procedure which included (1) acid digestion of resin samples in HNO 3 /HClO 4 , (2) radioactive decontamination by selective iodine extraction using a new chromatographic resin (CL Resin), and (3) AgI precipitation. Measured 129 I concentrations ranged from 4 to 12 ng/g, i.e. from 0.03 to 0.08 Bq/g. The calculation of 129 I/ 137 Cs activity ratios used for routine waste management produced values in agreement with the few available data for PWR resin samples. - Highlights: • In the context of radioactive waste management, this study aimed at measuring 129 I in spent resins using accelerator mass spectrometry. • The treatment procedure included microwave acid digestion of samples, iodine extraction by CL resins and AgI precipitation. • Developed first on synthetic matrices, the chemical treatment procedure was then successfully applied to real resin samples. • 129 I concentrations ranged from 4 to 12 ng/g of dry resin. • Results are in agreement with previous measurements and support reference values currently used for nuclear resin management

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.

Calculation of “LS-curves” for coincidence summing corrections in gamma ray spectrometry

Science.gov (United States)

Vidmar, Tim; Korun, Matjaž

2006-01-01

When coincidence summing correction factors for extended samples are calculated in gamma-ray spectrometry from full-energy-peak and total efficiencies, their variation over the sample volume needs to be considered. In other words, the correction factors cannot be computed as if the sample were a point source. A method developed by Blaauw and Gelsema takes the variation of the efficiencies over the sample volume into account. It introduces the so-called LS-curve in the calibration procedure and only requires the preparation of a single standard for each sample geometry. We propose to replace the standard preparation by calculation and we show that the LS-curves resulting from our method yield coincidence summing correction factors that are consistent with the LS values obtained from experimental data.

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

Mapping of depleted uranium with in situ spectrometry and soil samples

International Nuclear Information System (INIS)

Shebell, P.; Reginatto, M.; Monetti, M.; Faller, S.; Davis, L.

1999-01-01

Depleted uranium (DU) has been developed in the past two decades as a highly effective material for armor penetrating rounds and vehicle shielding. There is now a growing interest in the defense community to determine the presence and extent of DU contamination quickly and with a minimum amount of intrusive sampling. We report on a new approach using deconvolution techniques to quantitatively map DU contamination in surface soil. This approach combines data from soil samples with data from in situ gamma-ray spectrometry measurements to produce an accurate and detailed map of DU contamination. Results of a field survey at the Aberdeen Proving Ground are presented. (author)

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)

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

Hitomi X-ray Observation of the Pulsar Wind Nebula G21.5$-$0.9

OpenAIRE

Hitomi Collaboration; Aharonian, Felix; Akamatsu, Hiroki; Akimoto, Fumie; Allen, Steven W.; Angelini, Lorella; Audard, Marc; Awaki, Hisamitsu; Axelsson, Magnus; Bamba, Aya; Bautz, Marshall W.; Blandford, Roger; Brenneman, Laura W.; Brown, Gregory V.; Bulbul, Esra

2018-01-01

We present results from the Hitomi X-ray observation of a young composite-type supernova remnant (SNR) G21.5$-$0.9, whose emission is dominated by the pulsar wind nebula (PWN) contribution. The X-ray spectra in the 0.8-80 keV range obtained with the Soft X-ray Spectrometer (SXS), Soft X-ray Imager (SXI) and Hard X-ray Imager (HXI) show a significant break in the continuum as previously found with the NuSTAR observation. After taking into account all known emissions from the SNR other than the...

Use of Airborne Gamma-Ray Spectrometry in case of emergency. Example of HELGA exercise - collaboration between France and Germany

International Nuclear Information System (INIS)

Guillot, L.

2004-01-01

Since Chernobyl accident, airborne gamma-ray spectrometry has been recognised as a useful tool to evaluate consequences of an accident over large areas. Nine European countries have capabilities to perform such measurements. Between 1996 and 2003, a collaboration between these teams was supported by European community. In 2002, an exercise involving airborne and ground-based measurements was organised in Scotland. This exercise demonstrated the ability of European countries to provide assistance to one of them in case of emergency. Since this project has been completed, the French and German team decided to continue a collaboration. The CEA team (France) went in Germany in 2003 to participate to a survey with the German team. In September 2004, an exercise including mapping of contaminated areas and orphan sources search is planned in France. Such actions are good opportunities to exchange technical information about the acquisition systems and operating procedures. It is also essential to improve the availability of teams to obtain comparable and compatible results. The AGRS (airborne gamma ray spectrometry) systems involved in this exercise will be described and compared in this paper. The capacity of teams to work in collaboration in various situation (orphan source search, contamination mapping) will be then evaluated. In particular, a European Radiometric and Spectrometry format defined during Eccomags project will be used to create a database of raw and processed data. The aim is to produce quickly composite maps with data recorded by different teams. A choice of results will be presented and an assessment of capability of teams to work in collaboration will be done. (author)

Accurate joint space quantification in knee osteoarthritis: a digital x-ray tomosynthesis phantom study

Science.gov (United States)

Sewell, Tanzania S.; Piacsek, Kelly L.; Heckel, Beth A.; Sabol, John M.

2011-03-01

The current imaging standard for diagnosis and monitoring of knee osteoarthritis (OA) is projection radiography. However radiographs may be insensitive to markers of early disease such as osteophytes and joint space narrowing (JSN). Relative to standard radiography, digital X-ray tomosynthesis (DTS) may provide improved visualization of the markers of knee OA without the interference of superimposed anatomy. DTS utilizes a series of low-dose projection images over an arc of +/-20 degrees to reconstruct tomographic images parallel to the detector. We propose that DTS can increase accuracy and precision in JSN quantification. The geometric accuracy of DTS was characterized by quantifying joint space width (JSW) as a function of knee flexion and position using physical and anthropomorphic phantoms. Using a commercially available digital X-ray system, projection and DTS images were acquired for a Lucite rod phantom with known gaps at various source-object-distances, and angles of flexion. Gap width, representative of JSW, was measured using a validated algorithm. Over an object-to-detector-distance range of 5-21cm, a 3.0mm gap width was reproducibly measured in the DTS images, independent of magnification. A simulated 0.50mm (+/-0.13) JSN was quantified accurately (95% CI 0.44-0.56mm) in the DTS images. Angling the rods to represent knee flexion, the minimum gap could be precisely determined from the DTS images and was independent of flexion angle. JSN quantification using DTS was insensitive to distance from patient barrier and flexion angle. Potential exists for the optimization of DTS for accurate radiographic quantification of knee OA independent of patient positioning.

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)

Burn up determination of IEAR-1 fuel elements by non destructive gamma ray spectrometry method

International Nuclear Information System (INIS)

Soares, A.J.

1977-01-01

Measurement of nuclear fuel burn up by non destructive gamma ray spectrometry is discussed, and results of such measurements, made at the Instituto de Energia Atomica (IEA), are given. Specifically, the burn up of an MTR (Material Testing Reactor) fuel element removed from the IEAR-1 swimming pool reactor in 1958 is evaluated from the measured Cs-137 activity, which gives a single 661,6 keV gamma ray. Due to the long decay time of the test element, no other fission decay product activity could be detected. Analysis of measurements, made with a 3'' x 3'' NaI(Tl) detector at 330 distinct points of the element, showed the total burn up to 3.3 +- -+ 0.8 mg. This is in agreement with a calculated value. As the maximum temperature of IEAR-1 fuel elements is of the order of 40 0 C, migration effects of Cs-137 was not considered, this being significant only at fuel temperature in excess of 1000 0 C [pt

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)

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

Detection limits should be a thing of the past in gamma-ray spectrometry in general as well as in neutron activation analysis

NARCIS (Netherlands)

Blaauw, Menno

2016-01-01

In gamma-ray spectrometry with high-resolution detectors, full-energy peaks are often to be detected by a peak-search algorithm, with a threshold for detection. Detection limits can be derived from this. Detection limits are often computed along with measured activities or concentrations. When an

Gamma-ray spectrometry of ultra low levels of radioactivity within the material screening program for the GERDA experiment.

Science.gov (United States)

Budjás, D; Gangapshev, A M; Gasparro, J; Hampel, W; Heisel, M; Heusser, G; Hult, M; Klimenko, A A; Kuzminov, V V; Laubenstein, M; Maneschg, W; Simgen, H; Smolnikov, A A; Tomei, C; Vasiliev, S I

2009-05-01

In present and future experiments in the field of rare events physics a background index of 10(-3) counts/(keV kg a) or better in the region of interest is envisaged. A thorough material screening is mandatory in order to achieve this goal. The results of a systematic study of radioactive trace impurities in selected materials using ultra low-level gamma-ray spectrometry in the framework of the GERDA experiment are reported.

Accurate X-Ray Spectral Predictions: An Advanced Self-Consistent-Field Approach Inspired by Many-Body Perturbation Theory.

Science.gov (United States)

Liang, Yufeng; Vinson, John; Pemmaraju, Sri; Drisdell, Walter S; Shirley, Eric L; Prendergast, David

2017-03-03

Constrained-occupancy delta-self-consistent-field (ΔSCF) methods and many-body perturbation theories (MBPT) are two strategies for obtaining electronic excitations from first principles. Using the two distinct approaches, we study the O 1s core excitations that have become increasingly important for characterizing transition-metal oxides and understanding strong electronic correlation. The ΔSCF approach, in its current single-particle form, systematically underestimates the pre-edge intensity for chosen oxides, despite its success in weakly correlated systems. By contrast, the Bethe-Salpeter equation within MBPT predicts much better line shapes. This motivates one to reexamine the many-electron dynamics of x-ray excitations. We find that the single-particle ΔSCF approach can be rectified by explicitly calculating many-electron transition amplitudes, producing x-ray spectra in excellent agreement with experiments. This study paves the way to accurately predict x-ray near-edge spectral fingerprints for physics and materials science beyond the Bethe-Salpether equation.

Spatially-Dependent Measurements of Surface and Near-Surface Radioactive Material Using In situ Gamma Ray Spectrometry (ISGRS) For Final Status Surveys

International Nuclear Information System (INIS)

J. A. Chapman, A. J. Boerner, E. W. Abelquist

2006-01-01

In-situ, high-resolution gamma-ray spectrometry (ISGRS) measurements were conducted at the Oak Ridge Institute for Science and Education ORISE field laboratory in Oak Ridge, Tennessee. The purpose of these tests was to provide analytical data for assessing how 'fit for use' this technology is for detecting discrete particles in soil

Spatially-Dependent Measurements of Surface and Near-Surface Radioactive Material Using In situ Gamma Ray Spectrometry (ISGRS) For Final Status Surveys

Energy Technology Data Exchange (ETDEWEB)

J. A. Chapman, A. J. Boerner, E. W. Abelquist

2006-11-15

In-situ, high-resolution gamma-ray spectrometry (ISGRS) measurements were conducted at the Oak Ridge Institute for Science and Education (ORISE) field laboratory in Oak Ridge, Tennessee. The purpose of these tests was to provide analytical data for assessing how “fit for use” this technology is for detecting discrete particles in soil.

X-ray emission spectroscopy. X-ray fluorescence

International Nuclear Information System (INIS)

Despujols, J.

1992-01-01

Principles of X-ray emission spectrometry are first recalled, then wave-length dispersive and energy dispersive X-ray fluorescence spectrometer are described. They are essentially designed for qualitative and quantitative analysis of elements (Z>10). Sample preparation, calibration, corrections, interferences, accuracy are reviewed. Examples of use in different industries are given. (71 refs.)

Quantitative analysis or rare earths by X-ray fluorescence spectrometry

International Nuclear Information System (INIS)

Taam, Isabel; Mantovano, J.L.; Gante, Valdir; Jesus, Camila S.

2013-01-01

Rare earths ores and compounds are of growing importance to the worldwide industry. Its applications range from raw material to catalysts, manufacturing of electronics and even super magnets. Therefore, the demand for quick and accurate quantitative analysis methods is continuously growing. Current quantification methods of rare earths involve the separation of these elements by ion exchange and liquid-liquid extraction prior to the analysis itself, processes both time and reagent consuming. In the present work, we propose a method that directly quantifies by XRF technique the following rare earths: La, Pr, Nd, Sm and Gd in a concentrated liquor whose matrix also contains Ca, Y, PO4, U and Th. We evaluated the analytical interference of each element present on the sample on X-rays spectrum. The studied samples are certified standards and the obtained results have been compared to EDTA titration results, an already well-established and widely trusted method.We also measured the matrix effect thus using a complex rare earths standard. Results show that quantification by XRF technique is as accurate as the results in dose titration with EDTA for the same elements, with the advantage of exempting the previous separation step from each rare earth and from other elements present in the matrix (such as U and Th). (author)

Benchmarking density-functional-theory calculations of rotational g tensors and magnetizabilities using accurate coupled-cluster calculations.

Science.gov (United States)

Lutnaes, Ola B; Teale, Andrew M; Helgaker, Trygve; Tozer, David J; Ruud, Kenneth; Gauss, Jürgen

2009-10-14

An accurate set of benchmark rotational g tensors and magnetizabilities are calculated using coupled-cluster singles-doubles (CCSD) theory and coupled-cluster single-doubles-perturbative-triples [CCSD(T)] theory, in a variety of basis sets consisting of (rotational) London atomic orbitals. The accuracy of the results obtained is established for the rotational g tensors by careful comparison with experimental data, taking into account zero-point vibrational corrections. After an analysis of the basis sets employed, extrapolation techniques are used to provide estimates of the basis-set-limit quantities, thereby establishing an accurate benchmark data set. The utility of the data set is demonstrated by examining a wide variety of density functionals for the calculation of these properties. None of the density-functional methods are competitive with the CCSD or CCSD(T) methods. The need for a careful consideration of vibrational effects is clearly illustrated. Finally, the pure coupled-cluster results are compared with the results of density-functional calculations constrained to give the same electronic density. The importance of current dependence in exchange-correlation functionals is discussed in light of this comparison.

Basics of Gamma Ray Detection

Energy Technology Data Exchange (ETDEWEB)

Stinnett, Jacob [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Venkataraman, Ram [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)

2017-09-13

The objective of this training is to explain the origin of x-rays and gamma rays, gamma ray interactions with matter, detectors and electronics used in gamma ray-spectrometry, and features of a gamma-ray spectrum for nuclear material that is safeguarded.

Software for nuclear spectrometry

International Nuclear Information System (INIS)

1998-10-01

The Advisory Group Meeting (AGM) on Software for Nuclear Spectrometry was dedicated to review the present status of software for nuclear spectrometry and to advise on future activities in this field. Because similar AGM and consultant's meetings had been held in the past; together with an attempt to get more streamlined, this AGM was devoted to the specific field of software for gamma ray spectrometry. Nevertheless, many of the issues discussed and the recommendations made are of general concern for any software on nuclear spectrometry. The report is organized by sections. The 'Summary' gives conclusions and recommendations adopted at the AGM. These conclusions and recommendations resulted from the discussions held during and after presentations of the scientific and technical papers. These papers are reported here in their integral form in the following Sections

SU-F-T-555: Accurate Stereotactic Cone TMRs Converted from PDDs Scanned with Ray Trace

International Nuclear Information System (INIS)

Li, H; Zhong, H; Qin, Y; Snyder, K; Chetty, I; Wen, N

2016-01-01

Purpose: To investigate whether the accuracy of TMRs for stereotactic cones converted from PDDs scanned with Ray Trace can be improved, when compared against the TMRs converted from the traditional PDDs. Methods: Ray Trace measurement in Sun Nuclear 3D Scanner is for accurate scan of small field PDDs. The system detects the center of field at two depths, for example, at 3 and 20 cm in our study, and then performs scan along the line passing the two centers. With both Ray Trace and the traditional method, PDDs for conical cones of 4, 5, 7.5, 10, 12.5, 15, and 17.5 mm diameter (jaws set to 5×5 cm) were obtained for 6X FFF and 10X FFF energies on a Varian Edge linac, using Edge detectors. The formalism of converting PDD to TMR given in Khan’s book (4th Edition, p.161) was applied. Sp values at dmax were obtained by measuring cone Scp and Sc. Continuous direct measurement of TMR by filling/draining water to/from the tank and spot measurement by moving the tank and detector were also performed with the same equipment, using 100 cm SDD. Results: For 6XFFF energy and all the cones, TMRs converted from Ray Trace were very close to the continuous and spot measurement, while TMRs converted from traditional PDDs had larger deviation. Along the central axis beyond dmax, 1.7% of TMR data points calculated from Ray Trace had more 3% deviation from measurement, with maximal deviation of 5.2%. Whereas, 34% of TMR points calculated from traditional PDDs had more than 3% deviation, with maximum of 5.7%. In this initial study, Ray Trace scans for 10XFFF beam were noisy, further measurement is warranted. Conclusion: The Ray Trace could improve the accuracy of PDDs measurement and the calculated TMRs for stereotactic cones, which was within 3% of the measured TMRs.

SU-F-T-555: Accurate Stereotactic Cone TMRs Converted from PDDs Scanned with Ray Trace

Energy Technology Data Exchange (ETDEWEB)

Li, H; Zhong, H; Qin, Y; Snyder, K; Chetty, I; Wen, N [Henry Ford Health System, Detroit, MI (United States)

2016-06-15

Purpose: To investigate whether the accuracy of TMRs for stereotactic cones converted from PDDs scanned with Ray Trace can be improved, when compared against the TMRs converted from the traditional PDDs. Methods: Ray Trace measurement in Sun Nuclear 3D Scanner is for accurate scan of small field PDDs. The system detects the center of field at two depths, for example, at 3 and 20 cm in our study, and then performs scan along the line passing the two centers. With both Ray Trace and the traditional method, PDDs for conical cones of 4, 5, 7.5, 10, 12.5, 15, and 17.5 mm diameter (jaws set to 5×5 cm) were obtained for 6X FFF and 10X FFF energies on a Varian Edge linac, using Edge detectors. The formalism of converting PDD to TMR given in Khan’s book (4th Edition, p.161) was applied. Sp values at dmax were obtained by measuring cone Scp and Sc. Continuous direct measurement of TMR by filling/draining water to/from the tank and spot measurement by moving the tank and detector were also performed with the same equipment, using 100 cm SDD. Results: For 6XFFF energy and all the cones, TMRs converted from Ray Trace were very close to the continuous and spot measurement, while TMRs converted from traditional PDDs had larger deviation. Along the central axis beyond dmax, 1.7% of TMR data points calculated from Ray Trace had more 3% deviation from measurement, with maximal deviation of 5.2%. Whereas, 34% of TMR points calculated from traditional PDDs had more than 3% deviation, with maximum of 5.7%. In this initial study, Ray Trace scans for 10XFFF beam were noisy, further measurement is warranted. Conclusion: The Ray Trace could improve the accuracy of PDDs measurement and the calculated TMRs for stereotactic cones, which was within 3% of the measured TMRs.

DISCOVERY OF X-RAY EMISSION FROM AND DISTANCE TO THE SUPERNOVA REMNANT G84.2-0.8

Energy Technology Data Exchange (ETDEWEB)

Leahy, Denis A.; Green, Kaylie S., E-mail: leahy@ucalgary.ca, E-mail: ksgreen@ucalgary.ca [Department of Physics and Astronomy, University of Calgary, Calgary, Alberta, T2N 1N4 (Canada)

2012-11-20

We analyze X-ray and radio observations of the supernova remnant G84.2-0.8. 1420 MHz atomic hydrogen (H I) line and radio continuum data yield H I absorption spectra and a new H I absorption distance of 5.8-6.2 kpc. Archival X-ray observations from ROSAT and Chandra which cover the area including G84.2-0.8 are analyzed to show extended X-ray emission from G84.2-0.8. Fits to X-ray spectra from Chandra, with the new H I distance of 5.8-6.2 kpc, are used to determine the Sedov parameters of the supernova remnant. G84.2-0.8 is large (16-18 pc radius), middle aged ({approx}9000 yr), expanding in low-density interstellar medium (0.02 cm{sup -3}), and consistent with a low explosion energy (0.8-6.5 Multiplication-Sign 10{sup 50} erg).

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)

X-ray induction of 6-thioguanine-resistant mutants in division arrested, G0/G1 phase Chinese hamster ovary cells

Energy Technology Data Exchange (ETDEWEB)

O' Neill, J.P.; Flint, K.B.

The cytotoxic and mutagenic effect of X-irradiation was determined with Chinese hamster ovary cells arrested in the G0/G1 phase of the cell cycle through 9 days incubation in serum-free medium. In comparison with exponential phase cultures, the arrested cells showed increased cytotoxicity and mutation induction over the dose range of 50-800 rad. Exponential cultures showed a linear mutant frequency-survival relationship while the arrested cells showed a biphasic linear relationship. A post irradiation holding period 24 h does not result in any change in the mutant frequency. The increased sensitivity of the arrested cells to the mutagenic effects of X-rays appears to be a cell-cycle phase phenomenon. Upon readdition of serum, the arrested cells re-enter the cell cycle in a synchronous manner, reaching S phase at 10-12 h. Cells irradiated at 5 h after serum addition, i.e. in G1, show a similar dose response for mutant frequency, while those irradiated at 10 h or later, i.e. in late G1, S or G2, show lower mutation induction. These observations are consistent with a chromosome interchange mechanism of mutation induction by X-rays, possibly through interactions between repairing regions of the DNA. Irradiation of cells in the G0/G1 phase allow more time for such interactions in the absence of semiconservative DNA replication. (orig.).

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)

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.

Simple circuit for precise measurement of live dead or clock time in gamma-ray spectrometry

International Nuclear Information System (INIS)

Hammer, W.; Sterlinski, S.

1976-01-01

The basic design features and characteristics of circuit are described in the paper. The circuit coupled to a multichannel analyser (MCA) enables one of times: live(Tsub(iota)), dead (Tsub(d)) or clock(Tsub(c)) to be measured precisely. Second one is measured by a built-in timer of MCA. Having the Tsub(c)/Tsub(iota) ratio and utilizing suitable mathematical formulas one can make the corrections for both main effects (dead-time and pile-up) which yield counting losses in gamma-ray spectrometry at high and/or variable activities. Two examples of the dead-time and pile-up corrections by using the new circuit are presented in this paper. (author)

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

Assessment of the equilibrium of Th-228 and Ra-228 by gamma-ray spectrometry in mangrove soils

International Nuclear Information System (INIS)

Paiva, Jose Daniel S.; Farias, Emerson E.G.; Franca, Elvis J. De

2015-01-01

The mangrove environment consists of soil containing high organic matter, characterized by the influence of continental and oceanic waters, relatively high concentrations of salts and exuberant vegetation. Mangroves also present high dynamics of chemical compound cycling, in which soils become quite relevant due to the influence of continental and oceanic sediments. Taking into account the different sources and transport of radionuclides within the mangrove environment, this study focused at the radioactive equilibrium of Thorium-232 series radionuclides, especially the Ra-228 and Thorium-228. For this, soil samples were collected in the crown projection of tree species from two mangroves located in the municipalities of Olinda/Recife and Rio Formoso, Pernambuco State, Brazil. The material was oven-dried and milled and test portions of 38 g were transferred to cylindrical vials and sealed. After 30 days, the natural radioactivity was measured during 80,000 seconds using High Resolution Gamma-Ray Spectrometry with a germanium detector of 2.2 keV of resolution at the 1,332 keV Co-60 photopeak. For Ra-228 determination, 911 keV gamma-ray line (Ac-228) were employed, while 238 keV (Pb-212) and 727 keV (Bi-212) were considered for estimating activity concentrations of Th-228. As a result, Ra-228 and Th 228 were in equilibrium since the activity concentrations (ranging from 35 Bq/kg to 50 Bq/kg) were not significantly different at the 95% confidence level. The results have confirmed that, even for environments of high dynamics such as mangroves, radioactive equilibrium of Th-228 and Ra-228 was kept, corroborating Th-232 determination in mangrove soils. (author)

Assessment of the equilibrium of Th-228 and Ra-228 by gamma-ray spectrometry in mangrove soils

Energy Technology Data Exchange (ETDEWEB)

Paiva, Jose Daniel S.; Farias, Emerson E.G.; Franca, Elvis J. De, E-mail: paivajds@gmail.com, E-mail: emersonemiliano@yahoo.com.br, E-mail: ejfranca@cnen.gov.br [Centro Regional de Ciencias Nucleares do Nordeste (CRCN-NE/CNEN-PE), Recife, PE (Brazil)

2015-07-01

The mangrove environment consists of soil containing high organic matter, characterized by the influence of continental and oceanic waters, relatively high concentrations of salts and exuberant vegetation. Mangroves also present high dynamics of chemical compound cycling, in which soils become quite relevant due to the influence of continental and oceanic sediments. Taking into account the different sources and transport of radionuclides within the mangrove environment, this study focused at the radioactive equilibrium of Thorium-232 series radionuclides, especially the Ra-228 and Thorium-228. For this, soil samples were collected in the crown projection of tree species from two mangroves located in the municipalities of Olinda/Recife and Rio Formoso, Pernambuco State, Brazil. The material was oven-dried and milled and test portions of 38 g were transferred to cylindrical vials and sealed. After 30 days, the natural radioactivity was measured during 80,000 seconds using High Resolution Gamma-Ray Spectrometry with a germanium detector of 2.2 keV of resolution at the 1,332 keV Co-60 photopeak. For Ra-228 determination, 911 keV gamma-ray line (Ac-228) were employed, while 238 keV (Pb-212) and 727 keV (Bi-212) were considered for estimating activity concentrations of Th-228. As a result, Ra-228 and Th 228 were in equilibrium since the activity concentrations (ranging from 35 Bq/kg to 50 Bq/kg) were not significantly different at the 95% confidence level. The results have confirmed that, even for environments of high dynamics such as mangroves, radioactive equilibrium of Th-228 and Ra-228 was kept, corroborating Th-232 determination in mangrove soils. (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)

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)

Spectrometry techniques for radioactivity measurements

International Nuclear Information System (INIS)

Anilkumar, S.

2016-01-01

The energy of the radiation emission following the nuclear decay is unique and the characteristic of the radio nuclide which undergoes decay. Thus measurement of the energy of the radiation offers a method of identifying the radio nuclides. The prime requirement of the energy measurement is a suitable detector which shows response proportional to the energy of the radiation rather than the presence of the radiation. The response from such detectors are suitably processed and distributed with respect to the signal strength which is proportional to incident energy. This distribution is normally referred as energy spectrum and is recorded in the multichannel analyser. The measurement of energy and intensity of radiation from the spectrum is called radiation spectrometry. Thus the radiation spectrometry allows the identification and quantification of radioactive isotopes in variety of matrices. The radiation spectrometry has now become a popular radioanalytical technique in wide area of nuclear fuel cycle programs. The popular spectrometry techniques commonly used for the radioactivity measurement and analysis are Alpha spectrometry, Gamma ray spectrometry and Beta spectrometry

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.

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.

Determination of trace elements in freshwater rotifers and ciliates by total reflection X-ray fluorescence spectrometry

Science.gov (United States)

Woelfl, S.; Óvári, M.; Nimptsch, J.; Neu, T. R.; Mages, M.

2016-02-01

Element determination in plankton is important for the assessment of metal contamination of aquatic environments. Until recently, it has been difficult to determine elemental content in rotifers or ciliates derived from natural plankton samples because of the difficulty in handling and separation of these fragile organisms. The aim of this study was to evaluate methods for separation of rotifers and large ciliates from natural plankton samples (μg range dry weight) and subsequent analysis of their elemental content using total-reflection X-ray fluorescence spectrometry (TXRF). Plankton samples were collected from different aquatic environments (three lakes, one river) in Chile, Argentina and Hungary. From one to eighty specimens of five rotifer species (Brachionus calyciflorus, Brachionus falcatus, Asplanchna sieboldii, Asplanchna sp., Philodina sp.) and four to twelve specimens of one large ciliate (Stentor amethystinus) were prepared according to the dry method originally developed for microcrustaceans, and analysed by TRXF following in situ microdigestion. Our results demonstrated that it possible to process these small and fragile organisms (individual dry mass: 0.17-9.39 μg ind- 1) via careful washing and preparation procedures. We found species-dependent differences of the element mass fractions for some of the elements studied (Cr, Mn, Fe, Ni, Cu, Zn, As, Pb), especially for Cu, Fe and Mn. One large rotifer species (A. sieboldii) also showed a negative correlation between individual dry weight and the element content for Pb, Ni and Cr. We conclude that our application of the in situ microdigestion-TRXF method is suitable even for rotifers and ciliates, greatly expanding the possibilities for use of plankton in biomonitoring of metal contamination in aquatic environments.

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.

The synergistic radiosensitizing effect of tirapazamine-conjugated gold nanoparticles on human hepatoma HepG2 cells under X-ray irradiation

Directory of Open Access Journals (Sweden)

Liu X

2016-07-01

Full Text Available Xi Liu,1–4 Yan Liu,1–4 Pengcheng Zhang,1–4 Xiaodong Jin,1–3 Xiaogang Zheng,1–4 Fei Ye,1–4 Weiqiang Chen,1–3 Qiang Li1–3 1Institute of Modern Physics, 2Key Laboratory of Heavy Ion Radiation Biology and Medicine, Chinese Academy of Sciences, 3Key Laboratory of Basic Research on Heavy Ion Radiation Application in Medicine, Gansu Province, Lanzhou, 4School of Life Science, University of Chinese Academy of Sciences, Beijing, People’s Republic of China Abstract: Reductive drug-functionalized gold nanoparticles (AuNPs have been proposed to enhance the damage of X-rays to cells through improving hydroxyl radical production by secondary electrons. In this work, polyethylene glycol-capped AuNPs were conjugated with tirapazamine (TPZ moiety, and then thioctyl TPZ (TPZs-modified AuNPs (TPZs-AuNPs were synthesized. The TPZs-AuNPs were characterized by transmission electron microscopy, ultraviolet-visible spectra, dynamic light scattering, and inductively coupled plasma mass spectrometry to have a size of 16.6±2.1 nm in diameter and a TPZs/AuNPs ratio of ~700:1. In contrast with PEGylated AuNPs, the as-synthesized TPZs-AuNPs exhibited 20% increment in hydroxyl radical production in water at 2.0 Gy, and 19% increase in sensitizer enhancement ratio at 10% survival fraction for human hepatoma HepG2 cells under X-ray irradiation. The production of reactive oxygen species in HepG2 cells exposed to X-rays in vitro demonstrated a synergistic radiosensitizing effect of AuNPs and TPZ moiety. Thus, the reductive drug-conjugated TPZs-AuNPs as a kind of AuNP radiosensitizer with low gold loading provide a new strategy for enhancing the efficacy of radiation therapy. Keywords: AuNPs, radiation enhancement, synergistic effect, human hepatoma cells, hydroxyl radical production

ACCURATE MODELING OF X-RAY EXTINCTION BY INTERSTELLAR GRAINS

International Nuclear Information System (INIS)

Hoffman, John; Draine, B. T.

2016-01-01

Interstellar abundance determinations from fits to X-ray absorption edges often rely on the incorrect assumption that scattering is insignificant and can be ignored. We show instead that scattering contributes significantly to the attenuation of X-rays for realistic dust grain size distributions and substantially modifies the spectrum near absorption edges of elements present in grains. The dust attenuation modules used in major X-ray spectral fitting programs do not take this into account. We show that the consequences of neglecting scattering on the determination of interstellar elemental abundances are modest; however, scattering (along with uncertainties in the grain size distribution) must be taken into account when near-edge extinction fine structure is used to infer dust mineralogy. We advertise the benefits and accuracy of anomalous diffraction theory for both X-ray halo analysis and near edge absorption studies. We present an open source Fortran suite, General Geometry Anomalous Diffraction Theory (GGADT), that calculates X-ray absorption, scattering, and differential scattering cross sections for grains of arbitrary geometry and composition

ACCURATE MODELING OF X-RAY EXTINCTION BY INTERSTELLAR GRAINS

Energy Technology Data Exchange (ETDEWEB)

Hoffman, John; Draine, B. T., E-mail: jah5@astro.princeton.edu, E-mail: draine@astro.princeton.edu [Princeton University Observatory, Peyton Hall, Princeton, NJ 08544-1001 (United States)

2016-02-01

Interstellar abundance determinations from fits to X-ray absorption edges often rely on the incorrect assumption that scattering is insignificant and can be ignored. We show instead that scattering contributes significantly to the attenuation of X-rays for realistic dust grain size distributions and substantially modifies the spectrum near absorption edges of elements present in grains. The dust attenuation modules used in major X-ray spectral fitting programs do not take this into account. We show that the consequences of neglecting scattering on the determination of interstellar elemental abundances are modest; however, scattering (along with uncertainties in the grain size distribution) must be taken into account when near-edge extinction fine structure is used to infer dust mineralogy. We advertise the benefits and accuracy of anomalous diffraction theory for both X-ray halo analysis and near edge absorption studies. We present an open source Fortran suite, General Geometry Anomalous Diffraction Theory (GGADT), that calculates X-ray absorption, scattering, and differential scattering cross sections for grains of arbitrary geometry and composition.

Geochemical interpretation of gamma-ray spectrometry images from the Achala granite (Cordoba, Argentina)

International Nuclear Information System (INIS)

Lopez, Luis E.

1998-01-01

Data of an old spectrometry gamma-ray survey carried out in the Sierras Pampeanas Range by the National Atomic Energy Commission (Argentina) were reprocessed to obtain a corrected digital archive. The geochemical interpretation of the 250 x 250 meters spectrometric grids from the Achala batholith area was based on the behaviour of the radioelements in a peraluminous magma. Spectrometric maps of potassium, uranium, thorium and their ratios were used. In particular, the Th grid was very useful to define the primary magmatic evolution of the granitoids. K and U correlate roughly with Th distribution. The observed positive correlation between Th and U is thought to be the result of surficial leaching of U from uraninite. Finally, U/Th ratio allows to determine both, the magmatic evolution of the rocks and the mineral phase responsible for U content. (author)

The analysis of thallium in geological materials by radiochemical neutron activation and x-ray fluorescence spectrometry: a comparison

Energy Technology Data Exchange (ETDEWEB)

McGoldrick, P J; Robinson, P [Tasmania Univ., Sandy Bay, TAS (Australia)

1994-12-31

Carrier-based radiochemical neutron activation (RNAA) is a precise and accurate technique for the analysis of Tl in geological materials. For about a decade, until the mid-80s, a procedure modified from Keays et al. (1974) was used at the University of Melbourne to analyse for Tl in a wide variety of geological materials. Samples of powdered rock weighing several hundred milligrams each were irradiated in HIFAR for between 12 hours and 1 week, and subsequently fused with a sodium hydroxide - sodium peroxide mixture and several milligrams of inactive Tl carrier. Following acid digestion of the fusion mixture anion exchange resin was used to separate Tl from the major radioactive rock constituents. The Tl was then stripped from the resin and purified as thallium iodide and a yield measured gravimetrically. Activity from {sup 204}Tl (a {beta}-emitter with a 3 8 year half-life) was measured and Tl determined by reference to pure chemical standards irradiated and processed along with the unkowns. Detection limits for the longer irradiations were about one part per billion. Precision was monitored by repeat analyses of `internal standard` rocks and was estimated to be about five to ten percent (one standard deviation). On the other hand, X-ray fluorescence spectrometry (XRF) was seen as an excellent cost-effective alternative for thallium analysis in geological samples, down to 1 ppm. 6 refs. 1 tab., 1 fig.

The analysis of thallium in geological materials by radiochemical neutron activation and x-ray fluorescence spectrometry: a comparison

Energy Technology Data Exchange (ETDEWEB)

McGoldrick, P.J.; Robinson, P. [Tasmania Univ., Sandy Bay, TAS (Australia)

1993-12-31

Carrier-based radiochemical neutron activation (RNAA) is a precise and accurate technique for the analysis of Tl in geological materials. For about a decade, until the mid-80s, a procedure modified from Keays et al. (1974) was used at the University of Melbourne to analyse for Tl in a wide variety of geological materials. Samples of powdered rock weighing several hundred milligrams each were irradiated in HIFAR for between 12 hours and 1 week, and subsequently fused with a sodium hydroxide - sodium peroxide mixture and several milligrams of inactive Tl carrier. Following acid digestion of the fusion mixture anion exchange resin was used to separate Tl from the major radioactive rock constituents. The Tl was then stripped from the resin and purified as thallium iodide and a yield measured gravimetrically. Activity from {sup 204}Tl (a {beta}-emitter with a 3 8 year half-life) was measured and Tl determined by reference to pure chemical standards irradiated and processed along with the unkowns. Detection limits for the longer irradiations were about one part per billion. Precision was monitored by repeat analyses of `internal standard` rocks and was estimated to be about five to ten percent (one standard deviation). On the other hand, X-ray fluorescence spectrometry (XRF) was seen as an excellent cost-effective alternative for thallium analysis in geological samples, down to 1 ppm. 6 refs. 1 tab., 1 fig.

Self-attenuation correction in the environmental sample gamma spectrometry; Correcao de auto-absorcao na espectrometria gama de amostras ambientais

Energy Technology Data Exchange (ETDEWEB)

Venturini, Luzia; Nisti, Marcelo B. [Instituto de Pesquisas Energeticas e Nucleares (IPEN), Sao Paulo, SP (Brazil)

1997-10-01

Self-attenuation corrections were calculated for gamma ray spectrometry of environmental samples with densities from 0.42 g/ml up to 1.59 g/ml, measured in Marinelli beakers and polyethylene flasks. These corrections are to be used when the counting efficiency is calculated for water measured in the same geometry. The model of Debertin for Marinelli beaker, numerical integration and experimental linear attenuation coefficients were used. (author). 3 refs., 4 figs., 6 tabs.

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 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

Imaging mass spectrometry statistical analysis.

Science.gov (United States)

Jones, Emrys A; Deininger, Sören-Oliver; Hogendoorn, Pancras C W; Deelder, André M; McDonnell, Liam A

2012-08-30

Imaging mass spectrometry is increasingly used to identify new candidate biomarkers. This clinical application of imaging mass spectrometry is highly multidisciplinary: expertise in mass spectrometry is necessary to acquire high quality data, histology is required to accurately label the origin of each pixel's mass spectrum, disease biology is necessary to understand the potential meaning of the imaging mass spectrometry results, and statistics to assess the confidence of any findings. Imaging mass spectrometry data analysis is further complicated because of the unique nature of the data (within the mass spectrometry field); several of the assumptions implicit in the analysis of LC-MS/profiling datasets are not applicable to imaging. The very large size of imaging datasets and the reporting of many data analysis routines, combined with inadequate training and accessible reviews, have exacerbated this problem. In this paper we provide an accessible review of the nature of imaging data and the different strategies by which the data may be analyzed. Particular attention is paid to the assumptions of the data analysis routines to ensure that the reader is apprised of their correct usage in imaging mass spectrometry research. Copyright © 2012 Elsevier B.V. All rights reserved.

A low-energy set-up for gamma-ray spectrometry of NORM tailored to the needs of a secondary smelting facility

OpenAIRE

Lutter, Guilome; Vandael Schreurs, Indy; Croymans, Tom; Schroeyers, Wouter; Schreurs, Sonja; Hult, Mikael; Marissens, Gert; Stroh, Heiko; Tzikaa, Faidra

2017-01-01

A measurement station dedicated for quantitative radiological characterisation of naturally occurring radio-nuclides in a metallurgical company and based on gamma-ray spectrometry was developed. The station is intended for performing quality control of final non-ferrous metal products and for radiological checks of incoming materials. A low-background point-contact HPGe-detector was used and the signal was split in two branches to enable collecting simultaneously spectra with high amplificati...

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

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

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

Characteristics and quality test of X-ray with CZT detector

International Nuclear Information System (INIS)

Rianto, Sugeng

2000-01-01

The study examines the use of direct measurements of x-ray spectra for testing the quality of x-ray beam by using a peltier-cooled CZT detector under different conditions. The typical calibration of the spectrometry system shows that the energy resolution of the system is 1,2 keV at 122 keV of 57 Co. The utilization CZT based spectrometer for assessing the quality of x-ray machine on its spectra show that the CZT could accurately measure the spectra at various kVp, m As and filtration, except at the kVp greater than 140 and m As higher than 2 without added filtration. A comparison of CZT with the field instruments showed that there is a reasonable agreement between the Keithley and CZT at lower energies regardless of filtration however at high energies there is a large difference.In contrast the discrepancy between the CZT and Nero increased at lower photon energies particularly for high filtration

Prediction of collision cross section and retention time for broad scope screening in gradient reversed-phase liquid chromatography-ion mobility-high resolution accurate mass spectrometry

DEFF Research Database (Denmark)

Mollerup, Christian Brinch; Mardal, Marie; Dalsgaard, Petur Weihe

2018-01-01

artificial neural networks (ANNs). Prediction was based on molecular descriptors, 827 RTs, and 357 CCS values from pharmaceuticals, drugs of abuse, and their metabolites. ANN models for the prediction of RT or CCS separately were examined, and the potential to predict both from a single model......Exact mass, retention time (RT), and collision cross section (CCS) are used as identification parameters in liquid chromatography coupled to ion mobility high resolution accurate mass spectrometry (LC-IM-HRMS). Targeted screening analyses are now more flexible and can be expanded for suspect...

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

Analysis of a Soluble (UreD:UreF:UreG)2 Accessory Protein Complex and its Interactions with Klebsiella aerogenes Urease by Mass Spectrometry

Science.gov (United States)

Farrugia, Mark A.; Han, Linjie; Zhong, Yueyang; Boer, Jodi L.; Ruotolo, Brandon T.; Hausinger, Robert P.

2013-01-01

Maturation of the nickel-containing urease of Klebsiella aerogenes is facilitated by the UreD, UreF, and UreG accessory proteins along with the UreE metallo-chaperone. A fusion of the maltose binding protein and UreD (MBP-UreD) was co-isolated with UreF and UreG in a soluble complex possessing a (MBP-UreD:UreF:UreG)2 quaternary structure. Within this complex a UreF:UreF interaction was identified by chemical cross-linking of the amino termini of its two UreF protomers, as shown by mass spectrometry of tryptic peptides. A pre-activation complex was formed by the interaction of (MBP-UreD:UreF:UreG)2 and urease. Mass spectrometry of intact protein species revealed a pathway for synthesis of the urease pre-activation complex in which individual hetero-trimer units of the (MBP-UreD:UreF:UreG)2 complex bind to urease. Together, these data provide important new insights into the structures of protein complexes associated with urease activation. PMID:23797863

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)

Probing the Composition, Assembly and Activity of Protein Molecular Machines using Native Mass Spectrometry

NARCIS (Netherlands)

van de Waterbeemd, M.J.

2017-01-01

Native mass spectrometry and mass spectrometry in general, are powerful analytical tools for studying proteins and protein complexes. Native mass spectrometry may provide accurate mass measurements of large macromolecular assemblies enabling the investigation of their composition and stoichiometry.

Ultra-sensitive radionuclide spectrometry. Radiometrics and mass spectrometry synergy

International Nuclear Information System (INIS)

Povinec, P.P.

2005-01-01

Recent developments in radiometrics and mass spectrometry techniques for ultra-sensitive analysis of radionuclides in the marine environment are reviewed. In the radiometrics sector the dominant development has been the utilization of large HPGe detectors in underground laboratories with anti-cosmic or anti-Compton shielding for the analysis of short and medium-lived radionuclides in the environment. In the mass spectrometry sector, applications of inductively coupled plasma mass spectrometry (ICP-MS) and accelerator mass spectrometry (AMS) for the analysis of long-lived radionuclides in the environment are the most important recent achievements. The recent developments do not only considerably decrease the detection limits for several radionuclides (up to several orders of magnitude), but they also enable to decrease sample volumes so that sampling, e.g., of the water column can be much easier and more effective. A comparison of radiometrics and mass spectrometry results for the analysis of radionuclides in the marine environment shows a reasonable agreement - within quoted uncertainties, for wide range of activities and different sample matrices analyzed. (author)

Accurate quantification of polycyclic aromatic hydrocarbons in dust samples using microwave-assisted solvent extraction combined with isotope-dilution mass spectrometry

International Nuclear Information System (INIS)

Itoh, Nobuyasu; Fushimi, Akihiro; Yarita, Takashi; Aoyagi, Yoshie; Numata, Masahiko

2011-01-01

Highlights: → We applied MAE-IDMS for accurate quantification of PAHs in dust samples. → Both partitioning and isotopic equilibria can be achieved using this technique. → MAE-IDMS can provide accurate concentrations even if extraction efficiencies were low. → Characteristics of samples strongly affected for low extraction efficiencies of PAHs. - Abstract: For accurate quantification of polycyclic aromatic hydrocarbons (PAHs) in dust samples, we investigated the use of microwave-assisted solvent extraction (MAE) combined with isotope-dilution mass spectrometry (IDMS) using deuterium-labelled PAHs (D-PAHs). Although MAE with a methanol/toluene mixture (1:3 by volume) at 160 deg. C for 40 min was best for extracting PAHs from tunnel dust among examined, the recovery yields of D-PAHs decreased with increasing molecular weight (<40% for MW ≥ 264; that of deuterium-labelled indeno[123-cd]pyrene (D-IcdP) was only 7.1%). Although the residues were extracted a second time, the observed concentrations did not change dramatically (<5%), and the recovery yields of heavier D-PAHs (i.e., MW ≥ 264) were approximately half of those of the first extract, including D-IcdP (3.4%). These results suggest that both partitioning and isotopic equilibria of PAHs and D-PAHs between sample and solvent were achieved for extractable heavier PAHs under the condition. Thus, the observed concentrations of PAHs obtained by MAE-IDMS were reasonable, even though recovery yields of D-PAHs were <50%. From the results of carbon analyses and extractable contents, lower recovery yields of D-PAHs from the tunnel dust were due to a large content of char with low extractable contents.

The application of energy-dispersive x-ray fluorescence spectrometry (EDXRF) to the analysis of cosmetic evidence in Indian nail polishes

International Nuclear Information System (INIS)

Misra, G.; Sawhney, K.J.S.; Lodha, G.S.; Mittal, V.K.; Sahota, H.S.

1992-01-01

The application of energy-dispersive x-ray fluorescence (EDXRF) spectrometry in the quantitative analysis of samples of Indian nail polishes of apparently similar shades from different manufacturers has been examined by evaluating the possibility of detecting spurious material which is marketed under the guise of a popular brand. On the basis of the number of elements detected, and from the ratios of particular elements [Fe/Ti,Fe/Cu,Ti/Cu] the results are very encouraging. (author)

The application of energy-dispersive x-ray fluorescence spectrometry (EDXRF) to the analysis of cosmetic evidence in Indian nail polishes

Energy Technology Data Exchange (ETDEWEB)

Misra, G. (Forensic Science Lab., Chandigarh (India)); Sawhney, K.J.S.; Lodha, G.S. (Nuclear Research Lab., Srinagar (India)); Mittal, V.K.; Sahota, H.S. (Punjabi Univ., Patiala (India). Dept. of Physics)

1992-05-01

The application of energy-dispersive x-ray fluorescence (EDXRF) spectrometry in the quantitative analysis of samples of Indian nail polishes of apparently similar shades from different manufacturers has been examined by evaluating the possibility of detecting spurious material which is marketed under the guise of a popular brand. On the basis of the number of elements detected, and from the ratios of particular elements (Fe/Ti,Fe/Cu,Ti/Cu) the results are very encouraging. (author).

Analysis of sample γ-spectrometry with mathematic simulating

International Nuclear Information System (INIS)

Guo Hongsheng; He Xijun; Peng Taiping; Yang Gaozhao; Wang Wenchuan; Feng Chun

2005-01-01

When a sample contains various energy γ-rays, its peak area records not only the events of optical-electronic effect but also the Compton scattering events of higher energy γ-rays. So the γ-ray intensity conducted by the peak area can not be gained. Using the anti-matrix method, the better results of analysis on the γ-spectrometry can be obtained. (authors)

Accurate mass analysis of ethanesulfonic acid degradates of acetochlor and alachlor using high-performance liquid chromatography and time-of-flight mass spectrometry

Science.gov (United States)

Thurman, E.M.; Ferrer, I.; Parry, R.

2002-01-01

Degradates of acetochlor and alachlor (ethanesulfonic acids, ESAs) were analyzed in both standards and in a groundwater sample using high-performance liquid chromatography-time-of-flight mass spectrometry with electrospray ionization. The negative pseudomolecular ion of the secondary amide of acetochlor ESA and alachlor ESA gave average masses of 256.0750??0.0049 amu and 270.0786??0.0064 amu respectively. Acetochlor and alachlor ESA gave similar masses of 314.1098??0.0061 amu and 314.1153??0.0048 amu; however, they could not be distinguished by accurate mass because they have the same empirical formula. On the other hand, they may be distinguished using positive-ion electrospray because of different fragmentation spectra, which did not occur using negative-ion electrospray.

The application of gamma-spectrometry to nuclear power plant (NPP) and environment

International Nuclear Information System (INIS)

Asgharizadeh, Farid.

1995-01-01

One of measuring systems is nuclear spectrometry, particularly Gamma-Ray Spectrometry, to measure and determine the radionuclide concentration within plant materials and environmental samples. There are four major applied techniques related to Nuclear Power Plant operation and environmental monitoring aspects. Some details about gamma ray spectrometry technique is discussed in chapter 2. The main emphasis is on the calculation of gamma-ray detector efficiency for different geometries, the minimum detectable activity concepts and dead-time correction. Also,some formula and relations are introduced. In chapter 3, the major applications of gamma-ray spectrometry for analysis of nuclear power plant and environmental samples are discussed. These applications are divided into four topics: Nuclear Fuel survey; based on the activity of fission products concentration in reactor coolant, two other applications are introduced: Fuel Burnup calculation and the calculation of rated activity of natural radionuclides in construction of materials which is the last and most important application: Measurement and determination of radionuclides activity concentr[[[[n in environmental samples is described through section 3.3 Sampling and measuring methods for research and monitoring aspects is evaluated. Some data about sample preparation methods such as pretreatment and solubilization procedures are presented. Quantitative chemical separations of trace constituents from complex sample materials invariably require meticulous work by an analytical chemist. The radiochemical separation deals with this subject. Instrumental aspects, relate to gamma-ray spectrometry, quality assurance, presentation and reporting of results are described. In the experimental part, determination of radionuclides concentration in sediment sample is presented

Performance of alpha spectrometry in the analysis of uranium isotopes in environmental and nuclear materials

International Nuclear Information System (INIS)

Carvalho, F.P.; Oliveira, J.M.

2009-01-01

The accuracy of alpha spectrometry in the determination of uranium isotopes at various concentrations levels and with various isotope ratios was tested in a round robin international intercomparison exercise. Results of isotope activity/mass and isotope mass ratios obtained by alpha spectrometry were accurate in a wide range of uranium masses and in isotopic ratios typical of depleted, natural, and low enriched uranium samples. Determinations by alpha spectrometry compared very satisfactorily in accuracy with those by mass spectrometry. For example, determination of U isotopes in natural uranium by alpha spectrometry agreed with mass spectrometry determinations at within ±1%. However, the 236 U isotope, particularly if present in activities much lower than 235 U, might not be determined accurately due to overlap in the alpha particle energies of these two uranium isotopes. (author)

Radon fixation for determination of {sup 224}Ra, {sup 226}Ra and {sup 228}Ra via gamma-ray spectrometry

Energy Technology Data Exchange (ETDEWEB)

Herranz, M. [Departamento Ingenieria Nuclear y Mecanica de Fluidos, E. S. Ingenieros de Bilbao - Universidad del Pais Vasco (UPV/EHU), Alda. Urquijo s/n, 48013 Bilbao (Spain)]. E-mail: inphesom@bi.ehu.es; Idoeta, R. [Departamento Ingenieria Nuclear y Mecanica de Fluidos, E. S. Ingenieros de Bilbao - Universidad del Pais Vasco (UPV/EHU), Alda. Urquijo s/n, 48013 Bilbao (Spain); Abelairas, A. [Departamento Ingenieria Nuclear y Mecanica de Fluidos, E. S. Ingenieros de Bilbao - Universidad del Pais Vasco (UPV/EHU), Alda. Urquijo s/n, 48013 Bilbao (Spain); Legarda, F. [Departamento Ingenieria Nuclear y Mecanica de Fluidos, E. S. Ingenieros de Bilbao - Universidad del Pais Vasco (UPV/EHU), Alda. Urquijo s/n, 48013 Bilbao (Spain)

2006-04-15

The aim of this work is the improvement of the procedure for the determination of radium isotopes activities in water, which is done through radiochemical separation and subsequent gamma-ray spectrometry. In addition, radon gas retention is studied using different activated carbon materials. The results of the IAEA Proficiency test: 'Determination of radium and uranium radionuclides in water' of December 2002 [IAEA, 2003. Analytical quality control services: determination of radium and uranium radionuclides in water. Preliminary Report, Seibersdorf] are considered for this work.

Multivariate statistical approximation of the in situ gamma-ray spectrometry of the State of Zacatecas, Mexico

International Nuclear Information System (INIS)

Lopez I, J. F.; Rios M, C.; Mireles G, F.; Saucedo A, S.; Davila R, I.; Pinedo, J.L.

2017-09-01

The environmental radioactivity evaluation is a key point in the assessment of the environmental quality. Through this, it can be found possible radioactive contamination, locate possible Uranium and Thorium deposits and evaluate the primordial isotopes concentration due to human activities. A radioactive map of the Zacatecas State, Mexico is under construction based on in situ gamma-ray spectrometry. The present work reports the results of the multivariate statistical approximation of the measured activity data. Based on Pearson correlation, the 228 Ac and 208 Tl activities are statistically significant, while the 214 Bi and 214 Pb activities are not statistically significant. These can be due to the existence or not of secular equilibrium in the Thorium and Uranium series. (Author)

Comprehensive and accurate tracking of carbon origin of LC-tandem mass spectrometry collisional fragments for 13C-MFA.

Science.gov (United States)

Kappelmann, Jannick; Klein, Bianca; Geilenkirchen, Petra; Noack, Stephan

2017-03-01

In recent years the benefit of measuring positionally resolved 13 C-labeling enrichment from tandem mass spectrometry (MS/MS) collisional fragments for improved precision of 13 C-Metabolic Flux Analysis ( 13 C-MFA) has become evident. However, the usage of positional labeling information for 13 C-MFA faces two challenges: (1) The mass spectrometric acquisition of a large number of potentially interfering mass transitions may hamper accuracy and sensitivity. (2) The positional identity of carbon atoms of product ions needs to be known. The present contribution addresses the latter challenge by deducing the maximal positional labeling information contained in LC-ESI-MS/MS spectra of product anions of central metabolism as well as product cations of amino acids. For this purpose, we draw on accurate mass spectrometry, selectively labeled standards, and published fragmentation pathways to structurally annotate all dominant mass peaks of a large collection of metabolites, some of which with a complete fragmentation pathway. Compiling all available information, we arrive at the most detailed map of carbon atom fate of LC-ESI-MS/MS collisional fragments yet, comprising 170 intense and structurally annotated product ions with unique carbon origin from 76 precursor ions of 72 metabolites. Our 13 C-data proof that heuristic fragmentation rules often fail to yield correct fragment structures and we expose common pitfalls in the structural annotation of product ions. We show that the positionally resolved 13 C-label information contained in the product ions that we structurally annotated allows to infer the entire isotopomer distribution of several central metabolism intermediates, which is experimentally demonstrated for malate using quadrupole-time-of-flight MS technology. Finally, the inclusion of the label information from a subset of these fragments improves flux precision in a Corynebacterium glutamicum model of the central carbon metabolism.

Digital approach to high rate gamma-ray spectrometry

Energy Technology Data Exchange (ETDEWEB)

Korolczuk, Stefan; Mianowski, Slawomir; Rzadkiewicz, Jacek; Sibczynski, Pawel; Swiderski, Lukasz; Szewinski, Jaroslaw; Zychor, Izabella [Narodowe Centrum Badan Jadrowych (NCBJ), 05-400 Otwock, (Poland)

2015-07-01

Basic concepts and preliminary results of creating high rate digital spectrometry system using efficient ADCs and latest FPGA are presented as well as a comparison with commercially available devices. The possibility to use such systems, coupled to scintillators, in plasma experiments is discussed. (authors)

Thorium determination by x-ray fluorescence spectrometry in simulated thorex process solutions

International Nuclear Information System (INIS)

Yamaura, M.; Matsuda, H.T.

1991-11-01

The X-ray fluorescence method for thorium determination in aqueous and organic (TBP/n-dodecane) solutions is described. The thin film technique for sample preparation and a suitable internal standard had been used. The best conditions for Thorium determination had been established studying some parameters as analytical line, internal standard, filter paper, paper geometry, sample volume and measurement conditions. With the established conditions, thorium was concentration range of to 200 g Th/L and in organic solutions (2-63g Th/L) with 1,5% of precision. The accuracy of the proposed method was 3% in aqueous and organic phases. The detection limit was 1,2μg thorium for aqueous solutions and 1,4μg for organic solutions. Uranium, fission products, corrosion products and Thorex reagent components were studied as interfering elements in the thorium analysis. The matrix effect was also studied using the Thorex process simulated solutions. Finally, the method was applied to thorium determination in irradiated thorium solutions with satisfactory results. (author)

Rapid accurate analysis of metal (oxide)-on-silica catalysts by atomic absorption spectrometry

NARCIS (Netherlands)

Jütte, B.A.H.G.; Heikamp, A.; Agterdenbos, J.

1979-01-01

The catalysts, which contain 10–60% copper, chromium, nickel and silicon, are decomposed in sealed Teflon-lined vessels and analyzed by atomic absorption spectrometry. Matrix matching and bracketing standards are applied. The RSD of a single determination is about 1% for all components.

X-ray photoelectron spectroscopy and time-of-flight secondary ion mass spectrometry characterization of aging effects on the mineral fibers treated with aminopropylsilane and quaternary ammonium compounds

DEFF Research Database (Denmark)

Zafar, Ashar; Schjødt-Thomsen, Jan; Sodhi, R.

2012-01-01

(PCA) was applied to the time-of-flight secondary ion mass spectrometry spectra, and an increase in the intensities of APS characteristic peaks were observed after aging. The observed increase in the signals of APS originates from underlying silanized fibers after the removal of the surfactant......X-ray photoelectron spectroscopy (XPS) and time-of-flight secondary ion mass spectrometry were used to investigate the aging effects on the aminopropylsilane (APS) and quaternary ammonium surfactant-treated mineral fibers. APS-coated mineral fiber samples were treated with cationic surfactant...

Accurate determination of bromine and iodine in medicinal plants by inductively coupled plasma-mass spectrometry after microwave-induced combustion

Science.gov (United States)

Nascimento, Mariele S.; Mendes, Ana Luiza G.; Henn, Alessandra S.; Picoloto, Rochele S.; Mello, Paola A.; Flores, Erico M. M.

2017-12-01

In this work, a method for the determination of bromine and iodine in medicinal plants by inductively coupled plasma mass spectrometry (ICP-MS) after digestion by microwave-induced combustion (MIC) was developed. Medicinal plants were pressed as pellets and combusted at 20 bar of oxygen. The suitability of absorbing solution (water, 50 mmol L- 1 (NH4)2CO3, 10 mmol L- 1, 25 mmol L- 1, 50 mmol L- 1 or 100 mmol L- 1 NH4OH) was evaluated and a reflux step of 5 min was applied after combustion. The accuracy of the proposed method was evaluated by using certified reference materials (CRMs) of apple leaves and peach leaves and also by spiked samples. Using 50 mmol L- 1 NH4OH as absorbing solution, recoveries close to 100% for bromine and iodine were obtained as well as a low relative standard deviation (5%). No statistical difference (t-test, 95% of confidence level) was observed between the values obtained by ICP-MS after MIC digestion and the certified values. One of the important advantages of the proposed method is that it allowed the use of a relatively high sample mass (1000 mg) of medicinal plant resulting in low limits of quantification (0.033 μg g- 1 and 0.003 μg g- 1 for Br and I, respectively). Blanks were always negligible and only diluted solutions were used, in agreement with current recommendations for analytical methods. A high digestion efficiency was achieved (> 99%) assuring quantitative results. The concentration of analytes in medicinal plants was in the range of 0.17 μg g- 1 to 53.1 μg g- 1 for Br and medicinal plants (125 μg g- 1).

Rapid determination of halogenes in milk by instrumental neutron activation analysis

International Nuclear Information System (INIS)

Alfassi, Z.B.; Lavi, N.

1985-01-01

The absolute concetrations of iodine, bromine and chlorine in milk were determined by epithermal neutron activation followed by high resolution gamma-ray spectrometry. Two kinds of milk commonly consumed in Israel were investigated. The concentration of iodine, bromine and chlorine were found to be 0.18-0.30 μg/ml, 2.02-2.85 μg/ml and 0.65 mg/ml, respectively. The method is fast, selective, accurate and highly sensitive. (author)

Accurate Mass GC/LC-Quadrupole Time of Flight Mass Spectrometry Analysis of Fatty Acids and Triacylglycerols of Spicy Fruits from the Apiaceae Family

Directory of Open Access Journals (Sweden)

Thao Nguyen

2015-12-01

Full Text Available The triacylglycerol (TAG structure and the regio-stereospecific distribution of fatty acids (FA of seed oils from most of the Apiaceae family are not well documented. The TAG structure ultimately determines the final physical properties of the oils and the position of FAs in the TAG molecule affects the digestion; absorption and metabolism; and physical and technological properties of TAGs. Fixed oils from the fruits of dill (Anethum graveolens, caraway (Carum carvi, cumin (Cuminum cyminum, coriander (Coriandrum sativum, anise (Pimpinella anisum, carrot (Daucus carota, celery (Apium graveolens, fennel (Foeniculum vulgare, and Khella (Ammi visnaga, all from the Apiaceae family, were extracted at room temperature in chloroform/methanol (2:1 v/v using percolators. Crude lipids were fractionated by solid phase extraction to separate neutral triacylglycerols (TAGs from other lipids components. Neutral TAGs were subjected to transesterification process to convert them to their corresponding fatty acids methyl esters (FAMES using 1% boron trifluoride (BF3 in methanol. FAMES were analyzed by gas chromatography-quadrupole time of flight (GC-QTOF mass spectrometry. Triglycerides were analyzed using high performance liquid chromatography-quadrupole time of flight (LC-QTOF mass spectrometry. Petroselinic acid was the major fatty acid in all samples ranging from 57% of the total fatty acids in caraway up to 82% in fennel. All samples contained palmitic (16:0, palmitoleic (C16:1n-9, stearic (C18:0, petroselinic (C18:1n-12, linoleic (C18:2n-6, linolinic (18:3n-3, and arachidic (C20:0 acids. TAG were analyzed using LC-QTOF for accurate mass identification and mass spectrometry/mass spectrometry (MS/MS techniques for regiospesific elucidation of the identified TAGs. Five major TAGs were detected in all samples but with different relative concentrations in all of the tested samples. Several other TAGs were detected as minor components and were present in some

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)

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)

Compton suppression gamma ray spectrometry

International Nuclear Information System (INIS)

Landsberger, S.; Iskander, F.Y.; Niset, M.; Heydorn, K.

2002-01-01

In the past decade there have been many studies to use Compton suppression methods in routine neutron activation analysis as well as in the traditional role of low level gamma ray counting of environmental samples. On a separate path there have been many new PC based software packages that have been developed to enhance photopeak fitting. Although the newer PC based algorithms have had significant improvements, they still suffer from being effectively used in weak gamma ray lines in natural samples or in neutron activated samples that have very high Compton backgrounds. We have completed a series of experiments to show the usefulness of Compton suppression. As well we have shown the pitfalls when using Compton suppression methods for high counting deadtimes as in the case of neutron activated samples. We have also investigated if counting statistics are the same both suppressed and normal modes. Results are presented in four separate experiments. (author)

Simulation approach to coincidence summing in {gamma}-ray spectrometry

Energy Technology Data Exchange (ETDEWEB)

Dziri, S., E-mail: samir.dziri@iphc.cnrs.fr [Groupe RaMsEs, Institut Pluridisciplinaire Hubert Curien (IPHC), University of Strasbourg, CNRS, IN2P3, UMR 7178, 23 rue de Loess, BP 28, 67037 Strasbourg Cedex 2 (France); Nourreddine, A.; Sellam, A.; Pape, A.; Baussan, E. [Groupe RaMsEs, Institut Pluridisciplinaire Hubert Curien (IPHC), University of Strasbourg, CNRS, IN2P3, UMR 7178, 23 rue de Loess, BP 28, 67037 Strasbourg Cedex 2 (France)

2012-07-15

Some of the radionuclides used for efficiency calibration of a HPGe spectrometer are subject to coincidence-summing (CS) and account must be taken of the phenomenon to obtain quantitative results when counting samples to determine their activity. We have used MCNPX simulations, which do not take CS into account, to obtain {gamma}-ray peak intensities that were compared to those observed experimentally. The loss or gain of a measured peak intensity relative to the simulated peak is attributed to CS. CS correction factors are compared with those of ETNA and GESPECOR. Application to a test sample prepared with known radionuclides gave values close to the published activities. - Highlights: Black-Right-Pointing-Pointer Coincidence summing occurs when the solid angle is increased. Black-Right-Pointing-Pointer The loss of counts gives rise to an approximative efficiency curves, this means a wrong quantitative data. Black-Right-Pointing-Pointer To overcome this problem we need mono-energetic source, otherwise, the MCNPX simulation allows by comparison with the experiment data to get the coincidence summing correction factors. Black-Right-Pointing-Pointer By multiplying these factors by the approximative efficiency, we obtain the accurate efficiency.

Processing of gamma-ray spectrometric logs

International Nuclear Information System (INIS)

Umiastowski, K.; Dumesnil, P.

1984-10-01

CEA (Commissariat a l'Energie Atomique) has developped a gamma-ray spectrometric tool, containing an analog-to-digital converter. This new tool permits to perform very precise uranium logs (natural gamma-ray spectrometry), neutron activation logs and litho-density logs (gamma-gamma spectrometric logs). Specific processing methods were developped to treate the particular problems of down-hole gamma-ray spectrometry. Extraction of the characteristic gamma-ray peak, even if they are superposed on the background radiation of very high intensity, is possible. This processing methode enables also to obtain geological informations contained in the continuous background of the spectrum. Computer programs are written in high level language for SIRIUS (VICTOR) and APOLLO computers. Exemples of uranium and neutron activation logs treatment are presented [fr

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)

TeV γ-ray observations of the young synchrotron-dominated SNRs G1.9+0.3 and G330.2+1.0 with H.E.S.S.

Science.gov (United States)

H.E.S.S. Collaboration; Abramowski, A.; Aharonian, F.; Benkhali, F. Ait; Akhperjanian, A. G.; Angüner, E.; Anton, G.; Balenderan, S.; Balzer, A.; Barnacka, A.; Becherini, Y.; Becker Tjus, J.; Bernlöhr, K.; Birsin, E.; Bissaldi, E.; Biteau, J.; Böttcher, M.; Boisson, C.; Bolmont, J.; Bordas, P.; Brucker, J.; Brun, F.; Brun, P.; Bulik, T.; Carrigan, S.; Casanova, S.; Cerruti, M.; Chadwick, P. M.; Chalme-Calvet, R.; Chaves, R. C. G.; Cheesebrough, A.; Chrétien, M.; Colafrancesco, S.; Cologna, G.; Conrad, J.; Couturier, C.; Cui, Y.; Dalton, M.; Daniel, M. K.; Davids, I. D.; Degrange, B.; Deil, C.; deWilt, P.; Dickinson, H. J.; Djannati-Ataï, A.; Domainko, W.; O'C. Drury, L.; Dubus, G.; Dutson, K.; Dyks, J.; Dyrda, M.; Edwards, T.; Egberts, K.; Eger, P.; Espigat, P.; Farnier, C.; Fegan, S.; Feinstein, F.; Fernandes, M. V.; Fernandez, D.; Fiasson, A.; Fontaine, G.; Förster, A.; Füßling, M.; Gajdus, M.; Gallant, Y. A.; Garrigoux, T.; Giavitto, G.; Giebels, B.; Glicenstein, J. F.; Grondin, M.-H.; Grudzińska, M.; Häffner, S.; Hahn, J.; Harris, J.; Heinzelmann, G.; Henri, G.; Hermann, G.; Hervet, O.; Hillert, A.; Hinton, J. A.; Hofmann, W.; Hofverberg, P.; Holler, M.; Horns, D.; Jacholkowska, A.; Jahn, C.; Jamrozy, M.; Janiak, M.; Jankowsky, F.; Jung, I.; Kastendieck, M. A.; Katarzyński, K.; Katz, U.; Kaufmann, S.; Khélifi, B.; Kieffer, M.; Klepser, S.; Klochkov, D.; Kluźniak, W.; Kneiske, T.; Kolitzus, D.; Komin, Nu.; Kosack, K.; Krakau, S.; Krayzel, F.; Krüger, P. P.; Laffon, H.; Lamanna, G.; Lefaucheur, J.; Lemière, A.; Lemoine-Goumard, M.; Lenain, J.-P.; Lennarz, D.; Lohse, T.; Lopatin, A.; Lu, C.-C.; Marandon, V.; Marcowith, A.; Marx, R.; Maurin, G.; Maxted, N.; Mayer, M.; McComb, T. J. L.; Méhault, J.; Meintjes, P. J.; Menzler, U.; Meyer, M.; Moderski, R.; Mohamed, M.; Moulin, E.; Murach, T.; Naumann, C. L.; de Naurois, M.; Niemiec, J.; Nolan, S. J.; Oakes, L.; Ohm, S.; Wilhelmi, E. de Oña; Opitz, B.; Ostrowski, M.; Oya, I.; Panter, M.; Parsons, R. D.; Arribas, M. Paz; Pekeur, N. W.; Pelletier, G.; Perez, J.; Petrucci, P.-O.; Peyaud, B.; Pita, S.; Poon, H.; Pühlhofer, G.; Punch, M.; Quirrenbach, A.; Raab, S.; Raue, M.; Reimer, A.; Reimer, O.; Renaud, M.; Reyes, R. de los; Rieger, F.; Rob, L.; Romoli, C.; Rosier-Lees, S.; Rowell, G.; Rudak, B.; Rulten, C. B.; Sahakian, V.; Sanchez, D. A.; Santangelo, A.; Schlickeiser, R.; Schüssler, F.; Schulz, A.; Schwanke, U.; Schwarzburg, S.; Schwemmer, S.; Sol, H.; Spengler, G.; Spies, F.; Stawarz, Ł.; Steenkamp, R.; Stegmann, C.; Stinzing, F.; Stycz, K.; Sushch, I.; Szostek, A.; Tavernet, J.-P.; Tavernier, T.; Taylor, A. M.; Terrier, R.; Tluczykont, M.; Trichard, C.; Valerius, K.; van Eldik, C.; van Soelen, B.; Vasileiadis, G.; Venter, C.; Viana, A.; Vincent, P.; Völk, H. J.; Volpe, F.; Vorster, M.; Vuillaume, T.; Wagner, S. J.; Wagner, P.; Ward, M.; Weidinger, M.; Weitzel, Q.; White, R.; Wierzcholska, A.; Willmann, P.; Wörnlein, A.; Wouters, D.; Zabalza, V.; Zacharias, M.; Zajczyk, A.; Zdziarski, A. A.; Zech, A.; Zechlin, H.-S.

2014-06-01

The non-thermal nature of the X-ray emission from the shell-type supernova remnants (SNRs) G1.9+0.3 and G330.2+1.0 is an indication of intense particle acceleration in the shock fronts of both objects. This suggests that the SNRs are prime candidates for very-high-energy (VHE; E > 0.1 TeV) γ-ray observations. G1.9+0.3, recently established as the youngest known SNR in the Galaxy, also offers a unique opportunity to study the earliest stages of SNR evolution in the VHE domain. The purpose of this work is to probe the level of VHE γ-ray emission from both SNRs and use this to constrain their physical properties. Observations were conducted with the H.E.S.S. (High Energy Stereoscopic System) Cherenkov Telescope Array over a more than six-year period spanning 2004-2010. The obtained data have effective livetimes of 67 h for G1.9+0.3 and 16 h for G330.2+1.0. The data are analysed in the context of the multiwavelength observations currently available and in the framework of both leptonic and hadronic particle acceleration scenarios. No significant γ-ray signal from G1.9+0.3 or G330.2+1.0 was detected. Upper limits (99 per cent confidence level) to the TeV flux from G1.9+0.3 and G330.2+1.0 for the assumed spectral index Γ = 2.5 were set at 5.6 × 10-13 cm-2 s-1 above 0.26 TeV and 3.2 × 10-12 cm-2 s-1 above 0.38 TeV, respectively. In a one-zone leptonic scenario, these upper limits imply lower limits on the interior magnetic field to BG1.9 ≳ 12 μG for G1.9+0.3 and to BG330 ≳ 8 μG for G330.2+1.0. In a hadronic scenario, the low ambient densities and the large distances to the SNRs result in very low predicted fluxes, for which the H.E.S.S. upper limits are not constraining.

Assessing sample attenuation parameters for use in low-energy efficiency transfer in gamma-ray spectrometry

International Nuclear Information System (INIS)

Bruggeman, M.; Verheyen, L.; Vidmar, T.; Liu, B.

2016-01-01

We present a numerical fitting method for transmission data that outputs an equivalent sample composition. This output is used as input to a generalised efficiency transfer model based on the EFFTRAN software integrated in a LIMS. The procedural concept allows choosing between efficiency transfer with a predefined sample composition or with an experimentally determined composition based on a transmission measurement. The method can be used for simultaneous quantification of low-energy gamma emitters like "2"1"0Pb, "2"4"1Am, "2"3"4Th in typical environmental samples. - Highlights: • New fitting method for experimentally determined attenuation coefficients. • Generalised efficiency transfer with EFFTRAN based on transmission measurements. • Method of generalized efficiency transfer integrated in LIMS. • Method applicable to gamma-ray spectrometry of environmental samples.

Measurement of natural gamma radiation in building materials from Thellar of Tiruvannamalai Dist, Tamilnadu, India by gamma ray spectrometry

International Nuclear Information System (INIS)

Raghu, Y.; Ravisankar, R.; Chandrasekararn, A.; Vijayagopal, P.; Venkatraman, B.

2016-01-01

The knowledge of natural radioactivity in building materials is an important aspect of or determining the amount of public exposure because people spend most of their time (about 80%) indoors. Further, the knowledge of this radioactivity is useful in setting the standards and national guidelines in regard to the international recommendations and in assessing the associated radiation hazard. In the present work, the concentrations of natural radionuclides were measured in four types of building materials from Thellar of Tiruvannamalai district, Tamilnadu, India using gamma-ray spectrometry and associated radiological hazards are calculated

Einstein Observatory survey of X-ray emission from solar-type stars - the late F and G dwarf stars

Energy Technology Data Exchange (ETDEWEB)

Maggio, A.; Sciortino, S.; Vaiana, G.S.; Majer, P.; Bookbinder, J.

1987-04-01

Results of a volume-limited X-ray survey of stars of luminosity classes IV and V in the spectral range F7-G9 observed with the Einstein Observatory are presented. Using survival analysis techniques, the stellar X-ray luminosity function in the 0.15-4.0 keV energy band for both single and multiple sources. It is shown that the difference in X-ray luminosity between these two classes of sources is consistent with the superposition of individual components in multiple-component systems, whose X-ray properties are similar to those of the single-component sources. The X-ray emission of the stars in our sample is well correlated with their chromospheric CA II H-K line emission and with their projected equatorial rotational velocity. Comparison of the X-ray luminosity function constructed for the sample of the dG stars of the local population with the corresponding functions derived elsewhere for the Hyades, the Pleiades, and the Orion Ic open cluster confirms that the level of X-ray emission decreases with stellar age. 62 references.

Einstein Observatory survey of X-ray emission from solar-type stars - The late F and G dwarf stars

Science.gov (United States)

Maggio, A.; Sciortino, S.; Vaiana, G. S.; Majer, P.; Bookbinder, J.

1987-01-01

Results of a volume-limited X-ray survey of stars of luminosity classes IV and V in the spectral range F7-G9 observed with the Einstein Observatory are presented. Using survival analysis techniques, the stellar X-ray luminosity function in the 0.15-4.0 keV energy band for both single and multiple sources. It is shown that the difference in X-ray luminosity between these two classes of sources is consistent with the superposition of individual components in multiple-component systems, whose X-ray properties are similar to those of the single-component sources. The X-ray emission of the stars in our sample is well correlated with their chromospheric CA II H-K line emission and with their projected equatorial rotational velocity. Comparison of the X-ray luminosity function constructed for the sample of the dG stars of the local population with the corresponding functions derived elsewhere for the Hyades, the Pleiades, and the Orion Ic open cluster confirms that the level of X-ray emission decreases with stellar age.

Gamma ray spectrometry: applications in uranium prospecting and environment

International Nuclear Information System (INIS)

Lopez, Luis E.

1999-01-01

The experience in the use of gamma spectrometry for uranium prospecting and for the determination of natural radiation background is described. The basic principles of the techniques are also given. (author)

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.

Highly sensitive capillary electrophoresis-mass spectrometry for rapid screening and accurate quantitation of drugs of abuse in urine.

Science.gov (United States)

Kohler, Isabelle; Schappler, Julie; Rudaz, Serge

2013-05-30

The combination of capillary electrophoresis (CE) and mass spectrometry (MS) is particularly well adapted to bioanalysis due to its high separation efficiency, selectivity, and sensitivity; its short analytical time; and its low solvent and sample consumption. For clinical and forensic toxicology, a two-step analysis is usually performed: first, a screening step for compound identification, and second, confirmation and/or accurate quantitation in cases of presumed positive results. In this study, a fast and sensitive CE-MS workflow was developed for the screening and quantitation of drugs of abuse in urine samples. A CE with a time-of-flight MS (CE-TOF/MS) screening method was developed using a simple urine dilution and on-line sample preconcentration with pH-mediated stacking. The sample stacking allowed for a high loading capacity (20.5% of the capillary length), leading to limits of detection as low as 2 ng mL(-1) for drugs of abuse. Compound quantitation of positive samples was performed by CE-MS/MS with a triple quadrupole MS equipped with an adapted triple-tube sprayer and an electrospray ionization (ESI) source. The CE-ESI-MS/MS method was validated for two model compounds, cocaine (COC) and methadone (MTD), according to the Guidance of the Food and Drug Administration. The quantitative performance was evaluated for selectivity, response function, the lower limit of quantitation, trueness, precision, and accuracy. COC and MTD detection in urine samples was determined to be accurate over the range of 10-1000 ng mL(-1) and 21-1000 ng mL(-1), respectively. Copyright © 2013 Elsevier B.V. All rights reserved.

An accurate method for computer-generating tungsten anode x-ray spectra from 30 to 140 kV.

Science.gov (United States)

Boone, J M; Seibert, J A

1997-11-01

A tungsten anode spectral model using interpolating polynomials (TASMIP) was used to compute x-ray spectra at 1 keV intervals over the range from 30 kV to 140 kV. The TASMIP is not semi-empirical and uses no physical assumptions regarding x-ray production, but rather interpolates measured constant potential x-ray spectra published by Fewell et al. [Handbook of Computed Tomography X-ray Spectra (U.S. Government Printing Office, Washington, D.C., 1981)]. X-ray output measurements (mR/mAs measured at 1 m) were made on a calibrated constant potential generator in our laboratory from 50 kV to 124 kV, and with 0-5 mm added aluminum filtration. The Fewell spectra were slightly modified (numerically hardened) and normalized based on the attenuation and output characteristics of a constant potential generator and metal-insert x-ray tube in our laboratory. Then, using the modified Fewell spectra of different kVs, the photon fluence phi at each 1 keV energy bin (E) over energies from 10 keV to 140 keV was characterized using polynomial functions of the form phi (E) = a0[E] + a1[E] kV + a2[E] kV2 + ... + a(n)[E] kVn. A total of 131 polynomial functions were used to calculate accurate x-ray spectra, each function requiring between two and four terms. The resulting TASMIP algorithm produced x-ray spectra that match both the quality and quantity characteristics of the x-ray system in our laboratory. For photon fluences above 10% of the peak fluence in the spectrum, the average percent difference (and standard deviation) between the modified Fewell spectra and the TASMIP photon fluence was -1.43% (3.8%) for the 50 kV spectrum, -0.89% (1.37%) for the 70 kV spectrum, and for the 80, 90, 100, 110, 120, 130 and 140 kV spectra, the mean differences between spectra were all less than 0.20% and the standard deviations were less than approximately 1.1%. The model was also extended to include the effects of generator-induced kV ripple. Finally, the x-ray photon fluence in the units of

Multivariate statistical approximation of the in situ gamma-ray spectrometry of the State of Zacatecas, Mexico

Energy Technology Data Exchange (ETDEWEB)

Lopez I, J. F.; Rios M, C.; Mireles G, F.; Saucedo A, S.; Davila R, I.; Pinedo, J.L., E-mail: fernandolf498@gmail.com [Universidad Autonoma de Zacatecas, Unidad Academica de Estudios Nucleares, Cipres No. 10, Fracc. La Penuela, 98060 Zacatecas, Zac. (Mexico)

2017-09-15

The environmental radioactivity evaluation is a key point in the assessment of the environmental quality. Through this, it can be found possible radioactive contamination, locate possible Uranium and Thorium deposits and evaluate the primordial isotopes concentration due to human activities. A radioactive map of the Zacatecas State, Mexico is under construction based on in situ gamma-ray spectrometry. The present work reports the results of the multivariate statistical approximation of the measured activity data. Based on Pearson correlation, the {sup 228}Ac and {sup 208}Tl activities are statistically significant, while the {sup 214}Bi and {sup 214}Pb activities are not statistically significant. These can be due to the existence or not of secular equilibrium in the Thorium and Uranium series. (Author)

Rapid non-destructive quantitative estimation of urania/ thoria in mixed thorium uranium di-oxide pellets by high-resolution gamma-ray spectrometry

Energy Technology Data Exchange (ETDEWEB)

Shriwastwa, B.B.; Kumar, Anil; Raghunath, B.; Nair, M.R.; Abani, M.C.; Ramachandran, R.; Majumdar, S.; Ghosh, J.K

2001-06-01

A non-destructive technique using high-resolution gamma-ray spectrometry has been standardised for quantitative estimation of uranium/thorium in mixed (ThO{sub 2}-UO{sub 2}) fuel pellets of varying composition. Four gamma energies were selected; two each from the uranium and thorium series and the time of counting has been optimised. This technique can be used for rapid estimation of U/Th percentage in a large number of mixed fuel pellets from a production campaign.

Rapid non-destructive quantitative estimation of urania/ thoria in mixed thorium uranium di-oxide pellets by high-resolution gamma-ray spectrometry

International Nuclear Information System (INIS)

Shriwastwa, B.B.; Kumar, Anil; Raghunath, B.; Nair, M.R.; Abani, M.C.; Ramachandran, R.; Majumdar, S.; Ghosh, J.K.

2001-01-01

A non-destructive technique using high-resolution gamma-ray spectrometry has been standardised for quantitative estimation of uranium/thorium in mixed (ThO 2 -UO 2 ) fuel pellets of varying composition. Four gamma energies were selected; two each from the uranium and thorium series and the time of counting has been optimised. This technique can be used for rapid estimation of U/Th percentage in a large number of mixed fuel pellets from a production campaign

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

Application of gamma ray spectrometry and atomic absorption spectrometry for monitoring some radionuclides and heavy metals in sediments from the sudanese red sea coast

International Nuclear Information System (INIS)

Idris, A. M.; Eltayeb, M. A.

2004-01-01

A total of 31 surface sediment samples were collected from port-sudan harbour, sawakin harbour and the fringing reefs area that are located along the Sudanese coast of the red sea. The sampling was performed to provide good spatial coverage taking into account man's activity in port-sudan harbour and the fringing reefs area. the bulk samples were analyzed for some natural and anthropogenic radionuclides ( 226 Ra, 228 Ra, 40 K, 137 Cs) using direct gamma-ray spectrometry. Concentration of some heavy metals were determined in five fractions with grain-size of 1.000-0.500 m lm, 0.500-0.250 m lm, 0.250-0.125 m lm, 0.125-0.063 m lm and less than 0.063 m lm. The fractionation process was performed using dry sieving method. A total of 155 sub-samples (fractions) were digested by wet digestion method and analyzed for Mn, Fe, Ni, Cu, Zn, and Pb using flame atomic absorption spectrometry. Quality assurance of the obtained data was achieved through the analysis of certified reference materials. the radioactivity concentration ranges of ( 226 Ra, 228 Ra, and 40 K,) are 2.5-25.1b/kg, 2.1-13.1b q/kg,21.6- 429 Bq/kg, respectively. For ( 137 Cs)measurements, the highest value is 8.3 Bq/kg while most of samples were below the detection limits of the system. The concentration ranges of Mn, Fe, Cu, Zn, and Pb are 53.3-819 mg/kg, 1.4-51 mg/g, 8-131 mg/kg 9.5-113 mg/kg, 18.4-142 mg/kg, and 4.0-26.6 mg/kg, respectively. The granulometric normalization shows that some samples were subjected to anthropogenic activities. This finding was reinforced by results that were obtained from enrichment factor calculations and statistical multivariate analysis that is principal component analysis (Pca), also the Pca indicates that silt/clay fraction (>0.063 m lm ) is the dominant source for the emission of anthropogenic activities. From viewpoint of mineralogical composition the cluster analysis has distributed the samples into tow clusters. Dominant elements in sediments (Mn and Fe ) recorded

Joining X-Ray to Lensing: An Accurate Combined Analysis of MACS J0416.1–2403

Energy Technology Data Exchange (ETDEWEB)

Bonamigo, M.; Grillo, C. [Dark Cosmology Centre, Niels Bohr Institute, University of Copenhagen, Juliane Maries Vej 30, DK-2100 Copenhagen (Denmark); Ettori, S. [INAF, Osservatorio Astronomico di Bologna, Via Piero Gobetti, 93/3, 40129 Bologna (Italy); Caminha, G. B.; Rosati, P. [Dipartimento di Fisica e Scienze della Terra, Università degli Studi di Ferrara, Via Saragat 1, I-44122 Ferrara (Italy); Mercurio, A. [INAF—Osservatorio Astronomico di Capodimonte, Via Moiariello 16, I-80131 Napoli (Italy); Annunziatella, M. [INAF—Osservatorio Astronomico di Trieste, Via G.B. Tiepolo, 11 I-34143 Trieste (Italy); Balestra, I. [University Observatory Munich, Scheinerstrasse 1, D-81679 Munich (Germany); Lombardi, M., E-mail: bonamigo@dark-cosmology.dk [Dipartimento di Fisica, Università degli Studi di Milano, via Celoria 16, I-20133 Milano (Italy)

2017-06-20

We present a novel approach for a combined analysis of X-ray and gravitational lensing data and apply this technique to the merging galaxy cluster MACS J0416.1–2403. The method exploits the information on the intracluster gas distribution that comes from a fit of the X-ray surface brightness and then includes the hot gas as a fixed mass component in the strong-lensing analysis. With our new technique, we can separate the collisional from the collision-less diffuse mass components, thus obtaining a more accurate reconstruction of the dark matter distribution in the core of a cluster. We introduce an analytical description of the X-ray emission coming from a set of dual pseudo-isothermal elliptical mass distributions, which can be directly used in most lensing softwares. By combining Chandra observations with Hubble Frontier Fields imaging and Multi Unit Spectroscopic Explorer spectroscopy in MACS J0416.1–2403, we measure a projected gas-to-total mass fraction of approximately 10% at 350 kpc from the cluster center. Compared to the results of a more traditional cluster mass model (diffuse halos plus member galaxies), we find a significant difference in the cumulative projected mass profile of the dark matter component and that the dark matter over total mass fraction is almost constant, out to more than 350 kpc. In the coming era of large surveys, these results show the need of multiprobe analyses for detailed dark matter studies in galaxy clusters.

Preliminary Determination of Natural Radioactivity Levels of the State of Qatar using High-Resolution Gamma-ray Spectrometry

International Nuclear Information System (INIS)

Al-Sulaiti, H.A.; Regan, P.H.; Bradley, D.A.; Matthews, M.; Santawamaitre, T.; Malain, D.

2009-01-01

The State of Qatar is a peninsula with a total area of 11,437 km 2 which lies over a geological formation comprising a sequence of limestone, chalk, clay and gypsum. Establishing a baseline for the radioactivity concentration in Qatar's soil is the main purpose behind the present study. The project is focused on obtaining measurements of representative soil samples from various areas in Qatar to establish concentrations of the 235 U, 238 U and 232 Th natural decay chains and also the long-lived naturally occurring radionuclide 40 K. The 235 U, 238 U, 232 Th and 40 K concentrations have been measured via high-resolution gamma-ray spectrometry using a hyper-pure germanium detector situated in a low-background environment with a copper inner-plated passive lead shield. A wide range of different gamma-ray energy transitions lines arising from the multiple decay products from the 235 U, 238 U and 232 Th decay chains have been analyzed separately to obtain more statistically significant overall results

Hormesis of specific IgG antibody to rabies virus in serum of mice irradiated with low dose γ-rays

International Nuclear Information System (INIS)

Liu Qingjie; Chen Deqing

1998-01-01

Objective: To explore the effect of low dose ionizing radiation on specific antibody in mouse serum. Methods: Kunming strain male mice, weighing 18-22 g, aged 6-8 weeks, were immunized intraperitoneally with rabies vaccine after exposure to cobalt-60 γ-rays. The specific IgG antibody against rabies virus in mouse serum was measured. Results: (1) The serum levels of specific IgG in mice irradiated with 5-30 cGy γ-rays were significantly elevated in comparison with those in control mice (P<0.01), the optimum stimulating dose being 10 cGy. (2) Exposure to 10 cGy caused significant enhancement and earlier emergence of the peak level of specific IgG in serum. (3) The hormesis of specific IgG to rabies virus induced by 10 cGy γ-rays could last one week at least. Conclusion: Low dose ionizing radiation can enhance the level of specific antibody in mouse serum, and this effect can last for one week at least

Determination of mercury in seawater by total reflection x-ray fluorescence spectrometry after an electrochemical preconcentration method

International Nuclear Information System (INIS)

Ritschel, A.; Chinea Cano, E.; Wobrauschek, P.; Kuntner, C.; Durakbasa, M.N.

2000-01-01

A new combined method of electrodeposition of trace elements on metallic plates with subsequent total-reflection x-ray fluorescence spectrometry (TXRF) is proposed for the determination of trace metals in natural waters. The elements of interest are electroplated on highly polished niobium discs which are used as sample carriers for the TXRF measurement. The electrochemical preconcentration is performed in a flow cell under a controlled working electrode potential. The preconcentration step involves only very little manipulation which minimizes the risk of contamination of the sample. The method was investigated by analyzing inorganic mercury in sea water. A detection limit of 7 ngl -1 could be achieved for mercury in a 40 ml sea water sample. (author)

Inhibition pathways of the potent organophosphate CBDP with cholinesterases revealed by X-ray crystallographic snapshots and mass spectrometry

International Nuclear Information System (INIS)

Carletti, Eugenie; Santoni, Gianluca; Colletier, Jacques-Philippe; Schopfer, Lawrence M.; Lockridge, Oksana; Masson, Patrick; Nachon, Florian; Weik, Martin

2013-01-01

Tri-o-cresyl-phosphate (TOCP) is a common additive in jet engine lubricants and hydraulic fluids suspected to have a role in aero-toxic syndrome in humans. TOCP is metabolized to cresyl saligenin phosphate (CBDP), a potent irreversible inhibitor of butyrylcholinesterase (BChE), a natural bio-scavenger present in the bloodstream, and acetylcholinesterase (AChE), the off-switch at cholinergic synapses. Mechanistic details of cholinesterase (ChE) inhibition have, however, remained elusive. Also, the inhibition of AChE by CBDP is unexpected, from a structural standpoint, i.e., considering the narrowness of AChE active site and the bulkiness of CBDP. In the following, we report on kinetic X-ray crystallography experiments that provided 2.7-3.3 Angstroms snapshots of the reaction of CBDP with mouse AChE and human BChE. The series of crystallographic snapshots reveals that AChE and BChE react with the opposite enantiomers and that an induced-fit rearrangement of Phe297 enlarges the active site of AChE upon CBDP binding. Mass spectrometry analysis of aging in either H 2 16 O or H 2 18 O furthermore allowed us to identify the inhibition steps, in which water molecules are involved, thus providing insights into the mechanistic details of inhibition. X-ray crystallography and mass spectrometry show the formation of an aged end product formed in both AChE and BChE that cannot be reactivated by current oxime-based therapeutics. Our study thus shows that only prophylactic and symptomatic treatments are viable to counter the inhibition of AChE and BChE by CBDP. (authors)

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

Determination of plutonium isotopes in bilberry using liquid scintillation spectrometry and alpha-particle spectrometry

International Nuclear Information System (INIS)

Seferinoğlu, Meryem; Aslan, Nazife; Kurt, Aylin; Erden, Pınar Esra; Mert, Hülya

2014-01-01

This paper presents α-particle spectrometry and liquid scintillation spectrometry methods to determine plutonium isotopes in bilberry. The analytical procedure involves sample preparation steps for ashing, digestion of bilberry samples, radiochemical separation of plutonium radioisotopes and their measurement. The validity of the method was checked for coherence using the ζ test, z-test, relative bias and relative uncertainty outlier tests. The results indicated that the recommended procedures for both measurement systems could be successfully applied for the accurate determination of plutonium activities in bilberry samples. - Highlights: • Sample preparation methods for Pu using LSS and alpha spectrometry developed. • Complete separation of plutonium from interfering radionuclides. • Commercial bilberry was spiked with NPL 2011 (AH-B11144) proficiency test sample. • Results were checked using ζ test, z-test, rel. bias and rel. uncert. outlier tests. • Recommended procedures successfully applied to bilberry samples

Investigation of polyelectrolytes by total reflection x-ray fluorescence spectrometry

International Nuclear Information System (INIS)

Varga, I.; Nagy, M.

2000-01-01

Water soluble polyelectrolyte samples containing mono-, bi- and trivalent metal ions were investigated without any pretreatment. Acid digestion of linear polymers may lead to a product insoluble in water so the digestion has to be avoided. The aim of this paper was the determination of analytical characteristics and limitations of the total reflection x-ray fluorescence (TXRF) analysis for poly (vinylalcohol-vinylsulphate) salts and poly (acrylic acid, acrylamide) copolymers containing the following cations: K + , Cs + , Ba 2+ , Cu 2+ and La 3+ . On the basis of our results efficiency of ion-exchange during preparation of polyelectrolytes and stoichiometry of the end-product were determined. TXRF results were compared with data gained by inductively coupled plasma atomic emission spectrometry (ICP-AES) measurements except in the case of Cs + which has poor sensitivity in ICP-AES. Good agreement was found between the results of the two techniques and calculations from titrimetric data. Concentration of Li + and Mg 2+ in polymer samples was measured by ICP-AES. In majority of cases film-like dry residues of aqueous solutions of polyelectrolytes can be characterized by homogeneous spatial distribution of metal ions within the organic matrix. This is because the migration of the ions is hindered during drying process. Determination of metals in polyelectrolyte films by TXRF is quite ideal as model for analysis of plant, animal or human tissues which is a frequent task in environmental and inorganic biomedical analytical chemistry. (author)

High resolution gamma-ray spectrometry of culverts containing transuranic waste at the Savannah River Site

International Nuclear Information System (INIS)

Hofstetter, K.J.; Sigg, R.

1990-01-01

A number of concrete culverts used to retrievably store drummed, dry, radioactive waste at the Savannah River Site (SRS), were suspected of containing ambiguous quantities of transuranic (TRU) nuclides. These culverts were assayed in place for Pu-239 content using thermal and fast neutron counting techniques. High resolution gamma-ray spectroscopy on 17 culverts, having neutron emission rates several times higher than expected, showed characteristic gamma-ray signatures of neutron emitters other than Pu-239 (e.g., Pu-238, Pu/Be, or Am/Be neutron sources). This study confirmed the Pu-239 content of the culverts with anomalous neutron rates and established limits on the Pu-239 mass in each of the 17 suspect culverts by in-field, non-intrusive gamma-ray measurements

Opticofiber photoacoustic spectrometry in single-ray two-cell grouping for analytical determination of actinoids in solutions of reprocessing

International Nuclear Information System (INIS)

Yin'kov, S.I.; Myasoedov, B.F.; Kikhara, T.; Fuine, S.; Maeda, M.

1996-01-01

Single-ray two-cell version of photoacoustic spectrometry with laser excitation (Laser Induced Photoacoustic Spectroscopy, LIPAS) for remote determination of actinoids ions in solutions is developed. The spectrometer characteristics were specified by means of uranium-containing solutions, including a great number of non-radioactive ions, the absorption bonds where of imitated the absorption of Pu(3) and Pu(4). The possibilities of the LIPAS technique were studied by analysis of ions, imitating plutonium within the range of 650-724 nm on synthetic solutions with high uranium(6) content and a great number of nonradioactive isotopes of fragmentation-type elements. 8 refs., 9 figs., 1 tab

Precise and accurate isotope ratio measurements by ICP-MS.

Science.gov (United States)

Becker, J S; Dietze, H J

2000-09-01

The precise and accurate determination of isotope ratios by inductively coupled plasma mass spectrometry (ICP-MS) and laser ablation ICP-MS (LA-ICP-MS) is important for quite different application fields (e.g. for isotope ratio measurements of stable isotopes in nature, especially for the investigation of isotope variation in nature or age dating, for determining isotope ratios of radiogenic elements in the nuclear industry, quality assurance of fuel material, for reprocessing plants, nuclear material accounting and radioactive waste control, for tracer experiments using stable isotopes or long-lived radionuclides in biological or medical studies). Thermal ionization mass spectrometry (TIMS), which used to be the dominant analytical technique for precise isotope ratio measurements, is being increasingly replaced for isotope ratio measurements by ICP-MS due to its excellent sensitivity, precision and good accuracy. Instrumental progress in ICP-MS was achieved by the introduction of the collision cell interface in order to dissociate many disturbing argon-based molecular ions, thermalize the ions and neutralize the disturbing argon ions of plasma gas (Ar+). The application of the collision cell in ICP-QMS results in a higher ion transmission, improved sensitivity and better precision of isotope ratio measurements compared to quadrupole ICP-MS without the collision cell [e.g., for 235U/238U approximately 1 (10 microg x L(-1) uranium) 0.07% relative standard deviation (RSD) vs. 0.2% RSD in short-term measurements (n = 5)]. A significant instrumental improvement for ICP-MS is the multicollector device (MC-ICP-MS) in order to obtain a better precision of isotope ratio measurements (with a precision of up to 0.002%, RSD). CE- and HPLC-ICP-MS are used for the separation of isobaric interferences of long-lived radionuclides and stable isotopes by determination of spallation nuclide abundances in an irradiated tantalum target.

Simultaneous determination of RA-226, natural uranium and natural thorioum by gamma-ray spectrometry INa(Tl) in solid samples

International Nuclear Information System (INIS)

Salvador, S.; Navarro, T.; Alvarez, A.

1990-01-01

A method has been described to determine activities of Ra-226, natural uranium, and natural thorium, by gamma-ray spectrometry. The system was calibrated for efficiency by using synthetic calibrated standards. It is necessary, in the samples, to assume secular equilibrium between Ra-226 and Th-232 and its daughters nuclides, and U-238 and its immediate daughter Th-234, because the photopeaks measured are from these dsaugthers. Our results indicate that a non destructive gamma spectrometric method can ofter replace the radiochemical techniques used in measuring radiactivities in this type of samples. (Author). 9 refs

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)

Calculation of accurate small angle X-ray scattering curves from coarse-grained protein models

Directory of Open Access Journals (Sweden)

Stovgaard Kasper

2010-08-01

Full Text Available Abstract Background Genome sequencing projects have expanded the gap between the amount of known protein sequences and structures. The limitations of current high resolution structure determination methods make it unlikely that this gap will disappear in the near future. Small angle X-ray scattering (SAXS is an established low resolution method for routinely determining the structure of proteins in solution. The purpose of this study is to develop a method for the efficient calculation of accurate SAXS curves from coarse-grained protein models. Such a method can for example be used to construct a likelihood function, which is paramount for structure determination based on statistical inference. Results We present a method for the efficient calculation of accurate SAXS curves based on the Debye formula and a set of scattering form factors for dummy atom representations of amino acids. Such a method avoids the computationally costly iteration over all atoms. We estimated the form factors using generated data from a set of high quality protein structures. No ad hoc scaling or correction factors are applied in the calculation of the curves. Two coarse-grained representations of protein structure were investigated; two scattering bodies per amino acid led to significantly better results than a single scattering body. Conclusion We show that the obtained point estimates allow the calculation of accurate SAXS curves from coarse-grained protein models. The resulting curves are on par with the current state-of-the-art program CRYSOL, which requires full atomic detail. Our method was also comparable to CRYSOL in recognizing native structures among native-like decoys. As a proof-of-concept, we combined the coarse-grained Debye calculation with a previously described probabilistic model of protein structure, TorusDBN. This resulted in a significant improvement in the decoy recognition performance. In conclusion, the presented method shows great promise for

Overexpression, purification, crystallization and preliminary X-ray studies of Vibrio cholerae EpsG

International Nuclear Information System (INIS)

Jens, Jason; Raghunathan, Kannan; Vago, Frank; Arvidson, Dennis

2009-01-01

Recombinant V. cholerae EpsG has been expressed, purified and crystallized. The crystals diffracted to 2.26 Å resolution. EpsG is the major pseudopilin protein of the Vibrio cholerae type II secretion system. An expression plasmid that encodes an N-terminally truncated form of EpsG with a C-terminal noncleavable His tag was constructed. Recombinant EpsG was expressed in Escherichia coli; the truncated protein was purified and crystallized by hanging-drop vapor diffusion against a reservoir containing 6 mM zinc sulfate, 60 mM MES pH 6.5, 15% PEG MME 550. The crystals diffracted X-rays to a resolution of 2.26 Å and belonged to space group P2 1 , with unit-cell parameters a = 88.61, b = 70.02, c = 131.54 Å

The energy calibration and precision of a gamma spectrometry unit - Method using the electron annihilation energy as the only standard

International Nuclear Information System (INIS)

Hoclet, Michel

1971-06-01

Spectrometry using Ge(Li) detectors is discussed. The excellent resolution of this type of detector, the mathematical analysis of the spectral lines of the pulses, and the reproducibility of the spectrometer enable highly accurate measurements of the abscises (some 10 -5 ) corresponding to the peaks. A method using the annihilation energy of the electron as the only standard was developed. The method is applied to the measurement of the gamma ray energies of the radioelements: 22 Na, 24 Na, 56 Mn, 56 Co, 59 Fe, 72 Ga, 88 Y, 122 Sb, 124 Sb and 137 Cs. (author) [fr

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)

Optimization of chromatographic conditions for determination of aflatoxin B1, B2, G1 and G2 by using liquid chromatography-mass Spectrometry

Science.gov (United States)

Ramadhaningtyas, Dillani Putri; Aryana, Nurhani; Aristiawan, Yosi; Styarini, Dyah

2017-11-01

The optimization of instrument condition and chromatographic separation for analysis of aflatoxin B1, B2, G1 and G2 using liquid chromatography tandem with mass spectrometer detector was conducted in the aim to provide more accurate and reliable analysis results. The aflatoxin known to be serious threat for human health as it is classified as the carcinogenic compounds. The aflatoxin B1, B2, G1 and G2 were selected due to its extensive contamination in various agricultural commodities. The best chromatographic separation was obtained using C-18 column with gradient elution of solvent 5 mM ammonium acetate and 0.1% formic acid in methanol at 7 minutes runtime analysis. The linearity of the detector showed satisfied results as the coefficient determination found to be 0.9994, 0.9996, 0.9998 and 0.9987 for aflatoxin B1, G1, B2, and G2 respectively in the range concentration from 1 to 20 ng/g. The quantifier ion selected for the aflatoxin B1, B2, G1 and G2 was m/z 285.1, 259, 243 and 313 respectively. The instrument precision at these quantifier ions also showed satisfied result with %RSD was around 3.4 to 6.8%. The optimized method present in this study can be used for further sample analysis.

Effect of post-treatments with caffeine during G2 on the frequencies of chromosome-type aberrations produced by X-rays in human lymphocytes during G0 and G1

International Nuclear Information System (INIS)

Tanzarella, C.; De Salvia, R.; Degrassi, F.; Palitti, F.; Andersson, H.C.; Hansson, K.; Kihlman, B.A.

1986-01-01

Human lymphocytes were irradiated with X-rays in G 0 and G 1 , grown in the presence of 5-bromodeoxyuridine, and harvested at different times from 48 to 80 h after stimulation. Some cultures were exposed to 2.5-5 mM caffeine during the last 3 h before harvesting. The frequencies of chromosome-type aberrations were scored in first division (M 1 ) metaphases. The post-treatment with caffeine increased the frequencies of mitoses and chromosome-type aberrations in irradiated cultures. The results suggest that cells carrying chromosome-type aberrations are delayed in G 2 and that caffeine increases the frequencies of aberrations in dividing cells by removing this G 2 -block. (author)

Dispersive liquid-liquid microextraction and gas chromatography accurate mass spectrometry for extraction and non-targeted profiling of volatile and semi-volatile compounds in grape marc distillates.

Science.gov (United States)

Fontana, Ariel; Rodríguez, Isaac; Cela, Rafael

2018-04-20

The suitability of dispersive liquid-liquid microextraction (DLLME) and gas chromatography accurate mass spectrometry (GC-MS), based on a time-of-flight (TOF) MS analyzer and using electron ionization (EI), for the characterization of volatile and semi-volatile profiles of grape marc distillates (grappa) are evaluated. DLLME conditions are optimized with a selection of compounds, from different chemical families, present in the distillate spirit. Under final working conditions, 2.5 mL of sample and 0.5 mL of organic solvents are consumed in the sample preparation process. The absolute extraction efficiencies ranged from 30 to 100%, depending on the compound. For the same sample volume, DLLME provided higher responses than solid-phase microextraction (SPME) for most of the model compounds. The GC-EI-TOF-MS records of grappa samples were processed using a data mining non-targeted search algorithm. In this way, chromatographic peaks and accurate EI-MS spectra of sample components were linked. The identities of more than 140 of these components are proposed from comparison of their accurate spectra with those in a low resolution EI-MS database, accurate masses of most intense fragment ions of known structure, and available chromatographic retention index. The use of chromatographic and spectral data, associated to the set of components mined from different grappa samples, for multivariate analysis purposes is also illustrated in the study. Copyright © 2018 Elsevier B.V. All rights reserved.

Determination of natural radioactivity in building materials used in Tunisian dwellings by gamma ray spectrometry

International Nuclear Information System (INIS)

Hizem, N.; Fredj, A. B.; Ghedira, L.

2005-01-01

The radioisotopic content of 17 samples of natural and manufactured building materials collected in Tunisia have been analysed by using gamma spectrometry. From the measured gamma ray spectra, activity concentrations are determined for 232 Th, 226 Ra, 235 U and 40 K. The total effective dose and the activity concentration index are calculated applying the dose criteria recommended by the European Union for building materials. The results of 226 Ra, 232 Th and 40 K found in Tunisian building materials indicate that radium and thorium concentrations do not exceed 40 Bq kg -1 , but potassium concentration varies between 50 and 1215 Bq kg -1 . The total effective dose rates per person indoors are determined to be between 0.07 and 0.86 mSv y -1 . Only two materials exceed the reference level of 0.3 mSv y -1 . The activity concentration index is <1. (authors)

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.

Metabolic profiling of yeast culture using gas chromatography coupled with orthogonal acceleration accurate mass time-of-flight mass spectrometry: application to biomarker discovery.

Science.gov (United States)

Kondo, Elsuida; Marriott, Philip J; Parker, Rhiannon M; Kouremenos, Konstantinos A; Morrison, Paul; Adams, Mike

2014-01-07

Yeast and yeast cultures are frequently used as additives in diets of dairy cows. Beneficial effects from the inclusion of yeast culture in diets for dairy mammals have been reported, and the aim of this study was to develop a comprehensive analytical method for the accurate mass identification of the 'global' metabolites in order to differentiate a variety of yeasts at varying growth stages (Diamond V XP, Yea-Sacc and Levucell). Microwave-assisted derivatization for metabolic profiling is demonstrated through the analysis of differing yeast samples developed for cattle feed, which include a wide range of metabolites of interest covering a large range of compound classes. Accurate identification of the components was undertaken using GC-oa-ToFMS (gas chromatography-orthogonal acceleration-time-of-flight mass spectrometry), followed by principal component analysis (PCA) and orthogonal partial least squares discriminant analysis (OPLS-DA) for data reduction and biomarker discovery. Semi-quantification (fold changes in relative peak areas) was reported for metabolites identified as possible discriminative biomarkers (p-value 2), including D-ribose (four fold decrease), myo-inositol (five fold increase), L-phenylalanine (three fold increase), glucopyranoside (two fold increase), fructose (three fold increase) and threitol (three fold increase) respectively. Copyright © 2013 Elsevier B.V. All rights reserved.

Method Development for Rapid Analysis of Natural Radioactive Nuclides Using Sector Field Inductively Coupled Plasma Mass Spectrometry

Energy Technology Data Exchange (ETDEWEB)

Lim, J.M.; Ji, Y.Y.; Lee, H.; Park, J.H.; Jang, M.; Chung, K.H.; Kang, M.J.; Choi, G.S. [Korea Atomic Energy Research Institute (Korea, Republic of)

2014-07-01

As an attempt to reduce the social costs and apprehension arising from radioactivity in the environment, an accurate and rapid assessment of radioactivity is highly desirable. Naturally occurring radioactive materials (NORM) are widely spread throughout the environment. The concern with radioactivity from these materials has therefore been growing for the last decade. In particular, radiation exposure in the industry when handling raw materials (e.g., coal mining and combustion, oil and gas production, metal mining and smelting, mineral sands (REE, Ti, Zr), fertilizer (phosphate), and building materials) has been brought to the public's attention. To decide the proper handling options, a rapid and accurate analytical method that can be used to evaluate the radioactivity of radionuclides (e.g., {sup 238}U, {sup 235}U, {sup 232}Th, {sup 226}Ra, and {sup 40}K) should be developed and validated. Direct measuring methods such as alpha spectrometry, a liquid scintillation counter (LSC), and mass-spectrometry are usually used for the measurement of radioactivity in NORM samples, and they encounter the most significant difficulties during pretreatment (e.g., purification, speciation, and dilution/enrichment). Since the pretreatment process consequently plays an important role in the measurement uncertainty, method development and validation should be performed. Furthermore, a-spectrometry has a major disadvantage of a long counting time, while it has a prominent measurement capability at a very low activity level of {sup 238}U, {sup 235}U, {sup 232}Th, and {sup 226}Ra. Contrary to the α-spectrometry method, a measurement technique using ICP-MS allow radioactivity in many samples to be measured in a short time period with a high degree of accuracy and precision. In this study, a method was developed for a rapid analysis of natural radioactive nuclides using ICP-MS. A sample digestion process was established using LiBO{sub 2} fusion and Fe co-precipitation. A magnetic

Decay heat of 235U fission products by beta- and gamma-ray spectrometry

International Nuclear Information System (INIS)

Dickens, J.K.; Love, T.A.; McConnell, J.W.; Peelle, R.W.

1976-09-01

The fast-rabbit facilities of the ORRR were used to irradiate 1- to 10-μg samples of 235 U for 1, 10, and 100 s. Released power is observed using nuclear spectroscopy to permit separate observations of emitted β and γ spectra in successive time intervals. The spectra were integrated over energy to obtain total decay heat and the β- and γ-ray results are summed together. 10 fig, 2 tables

Immune response against antigens irradiated with 60Co gamma-rays

International Nuclear Information System (INIS)

Baptista, J.A.; Spencer, P.J.; Oliveira, J.E.; Casare, M.S.; Nascimento, N.

2006-01-01

In the present work, we investigated the immunological behavior of bothropstoxin-1, a K49 phospholipase from Bothrops jararacussu, and of ovalbumin before and after irradiation with 60 Co γ-rays. Isogenic mice were immunized with either native or irradiated proteins. The circulating antibodies were isotyped and titrated by ELISA. Results indicate that irradiated proteins were immunogenic and the antibodies elicited by them were able to recognize the native proteins in ELISA. Data also indicate that the irradiated protein induced higher titers of IgG2a and IgG2b, suggesting that Th1 cells were predominantly involved in the immune response. Structural modifications of the proteins were investigated by SDSPAGE, mass spectrometry and size exclusion chromatography. According to our data, irradiation promoted structural modifications on both proteins, characterized by higher molecular weight forms (aggregates and oligomers). When analyzed by mass spectrometry, the irradiated bothropstoxin appeared in several oxidized forms. These results indicate that irradiation of toxic proteins can promote significant modifications in their structures, but still retain many of the original antigenic and immunological properties of native form. (author)

In Vitro assessment of dentin erosion after immersion in acidic beverages: surface profile analysis and energy-dispersive X-ray fluorescence spectrometry study

OpenAIRE

Caneppele, Taciana Marco Ferraz; Jeronymo, Raffaela Di Iorio; Di Nicoló, Rebeca; Araújo, Maria Amélia Máximo de; Soares, Luís Eduardo Silva

2012-01-01

The aim of this study was to investigate the effects of some acidic drinks on dentin erosion, using methods of surface profile (SP) analysis and energy-dispersive X-ray fluorescence spectrometry (EDXRF). One hundred standardized dentin slabs obtained from bovine incisor roots were used. Dentin slabs measuring 5x5 mm were ground flat, polished and half of each specimen surface was protected with nail polish. For 60 min, the dentin surfaces were immersed in 50 mL of 5 different drinks (Gatorade...

NuSTAR study of hard X-ray morphology and spectroscopy of PWN G21.5-0.9

DEFF Research Database (Denmark)

Nynka, Melania; Hailey, Charles J.; Reynolds, Stephen P.

2014-01-01

We present NuSTAR high-energy X-ray observations of the pulsar wind nebula (PWN)/supernova remnant G21.5-0.9. We detect integrated emission from the nebula up to similar to 40 keV, and resolve individual spatial features over a broad X-ray band for the first time. The morphology seen by Nu...

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.

A broadband gamma-ray spectrometry using novel unfolding algorithms for characterization of laser wakefield-generated betatron radiation

Energy Technology Data Exchange (ETDEWEB)

Jeon, Jong Ho, E-mail: jhjeon07@ibs.re.kr; Nakajima, Kazuhisa, E-mail: naka115@dia-net.ne.jp; Pathak, Vishwa Bandhu; Cho, Myung Hoon; Yoo, Byung Ju; Shin, Kang Woo [Center for Relativistic Laser Science, Institute for Basic Science (IBS), Gwangju 500-712 (Korea, Republic of); Kim, Hyung Taek; Sung, Jae Hee; Lee, Seung Ku; Choi, Il Woo [Center for Relativistic Laser Science, Institute for Basic Science (IBS), Gwangju 500-712 (Korea, Republic of); Advanced Photonics Research Institute, GIST, Gwangju 500-712 (Korea, Republic of); Rhee, Yong Joo [Nuclear Data Center, Korea Atomic Energy Research Institute, Daejeon 305-353 (Korea, Republic of); Shin, Jung Hun; Jo, Sung Ha [Advanced Photonics Research Institute, GIST, Gwangju 500-712 (Korea, Republic of); Hojbota, Calin; Cho, Byeoung Ick; Nam, Chang Hee [Center for Relativistic Laser Science, Institute for Basic Science (IBS), Gwangju 500-712 (Korea, Republic of); Department of Physics and Photon Science, GIST, Gwangju 500-712 (Korea, Republic of)

2015-12-15

We present a high-flux, broadband gamma-ray spectrometry capable of characterizing the betatron radiation spectrum over the photon energy range from 10 keV to 20 MeV with respect to the peak photon energy, spectral bandwidth, and unique discrimination from background radiations, using a differential filtering spectrometer and the unfolding procedure based on the Monte Carlo code GEANT4. These properties are experimentally verified by measuring betatron radiation from a cm-scale laser wakefield accelerator (LWFA) driven by a 1-PW laser, using a differential filtering spectrometer consisting of a 15-filter and image plate stack. The gamma-ray spectra were derived by unfolding the photostimulated luminescence (PSL) values recorded on the image plates, using the spectrometer response matrix modeled with the Monte Carlo code GEANT4. The accuracy of unfolded betatron radiation spectra was assessed by unfolding the test PSL data simulated with GEANT4, showing an ambiguity of less than 20% and clear discrimination from the background radiation with less than 10%. The spectral analysis of betatron radiation from laser wakefield-accelerated electron beams with energies up to 3 GeV revealed radiation spectra characterized by synchrotron radiation with the critical photon energy up to 7 MeV. The gamma-ray spectrometer and unfolding method presented here facilitate an in-depth understanding of betatron radiation from LWFA process and a novel radiation source of high-quality photon beams in the MeV regime.

Matrix-assisted laser desorption/ionization-time of flight mass spectrometry identification of large colony beta-hemolytic streptococci containing Lancefield groups A, C, and G

DEFF Research Database (Denmark)

Salgård Jensen, Christian; Dam-Nielsen, Casper; Arpi, Magnus

2015-01-01

BACKGROUND: The aim of this study was to investigate whether large colony beta-hemolytic streptococci containing Lancefield groups A, C, and G can be adequately identified using matrix-assisted laser desorption/ionization-time of flight mass spectrometry (MALDI-ToF). Previous studies show varying...

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

The determination of major and some minor constituents in lead zirconate-titanate compositions by x-ray fluorescence and atomic absorption spectrometry

NARCIS (Netherlands)

van Willigen, J.H.H.G.; Kruidhof, H.; Dahmen, E.A.M.F.

1972-01-01

An accurate X-ray fluorescence spectrometric method is described for the determination of lead, zirconium and titanium in lead zirconate-titanate ceramics. Careful matching of samples and standards by a borax fusion method resulted in a relative standard deviation of about 0.2% for the major

Natural radioactivity in extreme south of Bahia, Brazil, using gamma-ray spectrometry

International Nuclear Information System (INIS)

Vasconcelos, Danilo C.; Oliveira, Arno H.; Silva, Mario R.S.; Penna, Rodrigo; Santos, Talita O.; Pereira, Claubia; Rocha, Zildete; Menezes, Maria Angela B.C.

2009-01-01

The concentrations activity of natural radionuclides in beach sand in extreme south of Bahia-Brazil was measured using gamma-ray spectrometry. The activity concentrations of 226 Ra, 232 Th and 40 K in beach sand ranged from 14.5 to 8,318.4, 20.5 to 18,450.0, 15.4 to 3,109.0 Bq/kg, with a mean value of 1,078.2, 2,429.6, and 417.0 Bq/kg respectively. The values of radiation hazard indexes in sands of Alcobaca, Caraiva and Cumuruxatiba are higher than the limits preconized by Beretka and Mathew. The use of these sands may be not safe in building constructions. The results show that the absorbed dose rates range from 20.4-15,116.6 nGy/h with mean value of 1762.7. The highest value of gamma dose rates among the studied beaches was found in Cumuruxatiba (15,116.6 nGy/h). The annual effective dose varied between 0.028 and 18.539 mSv/year, with a mean of 2.162 mSv/year. Values of Alcobaca, Trancoso, Caraiva and Cumuruxatiba are higher than the worldwide average for outdoor annual effective dose, 0.07 mSv/year. (author)

The application of computer technique in routine neutron activation analysis using high resolution gamma ray spectrometry

International Nuclear Information System (INIS)

Szopa, Z.; Plejewska, M.; Staszelis, J.

1982-01-01

A full system of four computer programs for routine - qualitative and quantitative - neutron activation analysis (NAA) using high resolution gamma ray-spectrometry had been elaborated. The structure and possibilities of the ''data flow'' programs i.e. programs DIDPDP and DIDCDC, dedicated for fast and reliable ''off line'' data transfer between the buffer memory of the spectrometric line (9-track magnetic tape) and the fast access memory (disc) of the used computers PDP-11/45 and CYBER-73 had been presented. The structure and organization of the ''data processing'' programs i.e. programs SAWAPS and MAZYG had been presented as well. The utility and reliability of these programs in the case of the large-scale, routine NAA, exampled by analysis of filters with air polutants, had been tested and discussed. Programs are written mainly in FORTRAN. (author)

Electronic structure of the dilute magnetic semiconductor G a1 -xM nxP from hard x-ray photoelectron spectroscopy and angle-resolved photoemission

Science.gov (United States)

Keqi, A.; Gehlmann, M.; Conti, G.; Nemšák, S.; Rattanachata, A.; Minár, J.; Plucinski, L.; Rault, J. E.; Rueff, J. P.; Scarpulla, M.; Hategan, M.; Pálsson, G. K.; Conlon, C.; Eiteneer, D.; Saw, A. Y.; Gray, A. X.; Kobayashi, K.; Ueda, S.; Dubon, O. D.; Schneider, C. M.; Fadley, C. S.

2018-04-01

We have investigated the electronic structure of the dilute magnetic semiconductor (DMS) G a0.98M n0.02P and compared it to that of an undoped GaP reference sample, using hard x-ray photoelectron spectroscopy (HXPS) and hard x-ray angle-resolved photoemission spectroscopy (HARPES) at energies of about 3 keV. We present experimental data, as well as theoretical calculations, to understand the role of the Mn dopant in the emergence of ferromagnetism in this material. Both core-level spectra and angle-resolved or angle-integrated valence spectra are discussed. In particular, the HARPES experimental data are compared to free-electron final-state model calculations and to more accurate one-step photoemission theory. The experimental results show differences between G a0.98M n0.02P and GaP in both angle-resolved and angle-integrated valence spectra. The G a0.98M n0.02P bands are broadened due to the presence of Mn impurities that disturb the long-range translational order of the host GaP crystal. Mn-induced changes of the electronic structure are observed over the entire valence band range, including the presence of a distinct impurity band close to the valence-band maximum of the DMS. These experimental results are in good agreement with the one-step photoemission calculations and a prior HARPES study of G a0.97M n0.03As and GaAs [Gray et al., Nat. Mater. 11, 957 (2012), 10.1038/nmat3450], demonstrating the strong similarity between these two materials. The Mn 2 p and 3 s core-level spectra also reveal an essentially identical state in doping both GaAs and GaP.

Chemical crosslinking and mass spectrometry studies of the structure and dynamics of membrane proteins and receptors.

Energy Technology Data Exchange (ETDEWEB)

Haskins, William E.; Leavell, Michael D.; Lane, Pamela; Jacobsen, Richard B.; Hong, Joohee; Ayson, Marites J.; Wood, Nichole L.; Schoeniger, Joseph S.; Kruppa, Gary Hermann; Sale, Kenneth L.; Young, Malin M.; Novak, Petr

2005-03-01

Membrane proteins make up a diverse and important subset of proteins for which structural information is limited. In this study, chemical cross-linking and mass spectrometry were used to explore the structure of the G-protein-coupled photoreceptor bovine rhodopsin in the dark-state conformation. All experiments were performed in rod outer segment membranes using amino acid 'handles' in the native protein sequence and thus minimizing perturbations to the native protein structure. Cysteine and lysine residues were covalently cross-linked using commercially available reagents with a range of linker arm lengths. Following chemical digestion of cross-linked protein, cross-linked peptides were identified by accurate mass measurement using liquid chromatography-fourier transform mass spectrometry and an automated data analysis pipeline. Assignments were confirmed and, if necessary, resolved, by tandem MS. The relative reactivity of lysine residues participating in cross-links was evaluated by labeling with NHS-esters. A distinct pattern of cross-link formation within the C-terminal domain, and between loop I and the C-terminal domain, emerged. Theoretical distances based on cross-linking were compared to inter-atomic distances determined from the energy-minimized X-ray crystal structure and Monte Carlo conformational search procedures. In general, the observed cross-links can be explained by re-positioning participating side-chains without significantly altering backbone structure. One exception, between C3 16 and K325, requires backbone motion to bring the reactive atoms into sufficient proximity for cross-linking. Evidence from other studies suggests that residues around K325 for a region of high backbone mobility. These findings show that cross-linking studies can provide insight into the structural dynamics of membrane proteins in their native environment.

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

Science.gov (United States)

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

2015-04-01

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

Field microcomputerized multichannel γ ray spectrometer based on notebook computer

International Nuclear Information System (INIS)

Jia Wenyi; Wei Biao; Zhou Rongsheng; Li Guodong; Tang Hong

1996-01-01

Currently, field γ ray spectrometry can not rapidly measure γ ray full spectrum, so a field microcomputerized multichannel γ ray spectrometer based on notebook computer is described, and the γ ray full spectrum can be rapidly measured in the field

Significance of radioelement concentration measurements made by airborne gamma-ray spectrometry over the Canadian Shield

International Nuclear Information System (INIS)

Charbonneau, B.W.; Killeen, P.G.; Carson, J.M.; Cameron, G.W.; Richardson, K.A.

1976-01-01

Results of airborne gamma-ray spectrometer surveys conducted by the Geological Survey of Canada are presented as maps contoured in units of radioelement and concentration ratios. These contoured values represent the average surface concentrations of the radioelements over areas of the order of several square kilometres. The relationship between this ''average surface concentration'' and the radioelement concentration in bedrock underlying the area depends on: (1) the percentage of outcrop; (2) the relation between overburden and bedrock radioelement concentration; (3) percentage of marshland or surface water in the area; (4) soil moisture; and (5) density of vegetation. More than 2500 portable gamma-ray spectrometer analyses of outcrop and overburden have been made in the Bancroft, Elliot Lake and Fort Smith areas of the Canadian Precambrian Shield. In the areas examined, the radioelement concentrations in glacial drift reflect the concentrations in the underlying bedrock. Rocks with near-crustal average contents of thorium, uranium and potassium are overlain by glacial drift having approximately the same concentrations. As the concentration in bedrock increases, the concentration in the local overburden also increases, but not to the same extent. In addition, in-situ gamma-ray spectrometry measurements were made at almost 1000 stations within the area of airborne surveys near Mont Laurier and Elliot Lake. These ground measurements were compared with the airborne measurements by averaging the values for all those ground stations located in the areas between each contour level on airborne maps. Radioelement concentrations in bedrock are considerably higher than corresponding airborne measurements, and this difference between bedrock and airborne values increases at higher radioelement concentrations. Radioelement concentrations in glacial drift are only slightly higher than airborne contour values for the same area. Airborne contour maps of the radioelement ratios

Theory of in situ gamma-ray spectrometry

International Nuclear Information System (INIS)

Balea, G.

2002-01-01

The technique of in situ spectrometry had its origin during the time of atmospheric nuclear weapons testing when is was found to provide quick, reliable information on the components of the outdoor environment. It provided a means to separate natural background from man-made sources and gave quantitative results. Over the years, it has been employed by various groups for assessing radiation sources in the environment not only via ground based detectors, but with aircraft systems as well. It proved particularly useful after the Chernobyl accident and was employed by a number of European laboratories. It should prove adaptable to site assessment in the current era of environmental rescue. (author)

Comparative studies for determining U-235/U-238 relation in solutions of natural and depleted uranium using gamma spectrometry and neutron activation analysis

International Nuclear Information System (INIS)

Cassorla F, V.; Valle M, L.; Pena V, L.

1988-01-01

Two experimental methods were developed for determining U-235/U-238 ratio in uranium solutions. The isotopic was measured by high resolution ratio gamma-ray spectrometry (G.S.) and neutron activation analysis (N.A.A.). The precision obtained was similar for both methods, but better sensitivity was obtained by N.A.A. The accuracy in both cases was stablished by comparison with samples previously analyzed by mass spectrometry, the results were satisfactory for both techniques. Studies involving the influence of the nitric acid concentration on the isotopic ratio measurement, also were done. In addition, computer programs for faster data reduction were developped, in the case of N.A.A. (author)

The determination of trace elements in commercial human serum albumin solutions by proton-induced X-ray emission spectrometry and neutron activation analysis

International Nuclear Information System (INIS)

Maenhaut, W.; De Reu, L.; Tomza, U.; Versieck, J.

1982-01-01

Particle induced X-ray emission (p.i.x.e.) and neutron activation analysis (n.a.a.) are proposed for determining the trace element content of human serum albumin. Application of these methods to some commercial albumin solutions provided concentration data for up to 19 elements, most of which were present at a level below a few μg ml -1 . The precision of the p.i.x.e. technique, as determined by irradiating up to 20 targets from one sample, was about 3% for those elements where counting statistics were good. A comparison between the p.i.x.e. and n.a.a. results showed close agreement, indicating that p.i.x.e. can yield data which are accurate to within 10%. Neutron activation showed very good sensitivity for the elements producing long-lived nuclides (tsub(1/2) >= 3 days), but had rather high detection limits for the other elements, unless radiochemical separations were used. (Auth.)

Advances in low atomic number element analysis by wavelength dispersive x-ray fluorescence spectrometry

International Nuclear Information System (INIS)

Vrebos, B.

1996-01-01

Traditionally, the analysis of low atomic number has been a chal1enging task for wavelength dispersive x-ray fluorescence spectrometry. Among the most important factors influencing analysis of the low atomic number elements (from Z=11 downwards) are the fluorescence yield, absorption and the dispersion. The effect of each of these factors on the overall performance will be illustrated. The long wavelengths involved (longer than I nm) used to pose severe problems concerning the monochromator used. Early instruments relied on lead stearate or Blodgett Langmuir soap films for the diffraction of the characteristic radiation. Nowadays, synthetic multilayers are commonly used. The performance of these multilayers is determined by the reflectivity, the resolution and the absorption of the characteristic radiation to be diffracted. These parameters can be optimised by adequately selecting the composition of the materials involved. The sensitivity of the modem instruments is sufficient to allow quantitative analysis. However, this aspect of WDS XRF is still met with considerable scepticism. Examples of quantitative analysis will be given to illustrate the current capability

Proton Induced X-Rays Emission (PIXE) and Atomic Absorption Spectrometry (AAS) applied in the environmental sample analysis

International Nuclear Information System (INIS)

Popescu, Ion V.; Iordan, M.; Stihi, C.; Bancuta, A.; Dima, G.; Busuioc, G.; Ciupina, V.; Belc, M.; Badica, T.

2003-01-01

The aim of this work is to determine the elemental composition of tree leaves using Proton-Induced X-Rays Emission (PIXE) and Atomic Absorption Spectrophotometry (AAS) methods. By PIXE Spectrometry we identified and determined the concentration of S, Cl, K, Ca, Ti, Cr, Mn, Fe, Co, Ni, Cu Zn, As, Br, Sr and by AAS method the concentration of elements: Cr, Mn, Fe, Co, Cu, Zn, Se, Cd. Pb was identified in only 2 samples from 29. For tree leave samples collected at a large distance to the polluting source the Sr concentration decreased and the Mg, Ca, Se, Zn and Fe concentrations increased. Also, we can observe a small affinity of these leaves for the environmental Pb which was detected for two samples at a small distance to polluting source. (authors)

40 K, 137 Cs and 232 Th activities in Brazilian milk samples measured by gamma ray spectrometry

International Nuclear Information System (INIS)

Melquiades, Fabio L.; Appoloni, Carlos R.

2000-01-01

This work deals with the measurement of radioactive activities in powdered milk, with high resolution gamma-ray spectrometry, using a HPGe detector coupled to a standard electronic nuclear chain and a multichannel card of 8192 channels. Preliminary measurements were accomplished to define the kind of the system shield, the geometry of the sample recipient, the size of the sampling and the self absorption correction. It was possible to measure the radionuclides 40 K, 137 Cs and 208 Tl, whose activities were calculated according to the International Atomic Energy Agency norms. The detector efficiency was measured employing calibrated samples, prepared with IAEA certificate standards mixed with powdered milk. Tukey's average comparison test was used to check the repeatability of the measurements and the absence of significant systematic deviation. (author)

DISCOVERY OF TeV GAMMA-RAY EMISSION TOWARD SUPERNOVA REMNANT SNR G78.2+2.1

Energy Technology Data Exchange (ETDEWEB)

Aliu, E. [Department of Physics and Astronomy, Barnard College, Columbia University, NY 10027 (United States); Archambault, S. [Physics Department, McGill University, Montreal, QC H3A 2T8 (Canada); Arlen, T.; Aune, T. [Department of Physics and Astronomy, University of California, Los Angeles, CA 90095 (United States); Beilicke, M.; Buckley, J. H.; Bugaev, V.; Dickherber, R. [Department of Physics, Washington University, St. Louis, MO 63130 (United States); Benbow, W. [Fred Lawrence Whipple Observatory, Harvard-Smithsonian Center for Astrophysics, Amado, AZ 85645 (United States); Bird, R.; Cannon, A.; Collins-Hughes, E. [School of Physics, University College Dublin, Belfield, Dublin 4 (Ireland); Bouvier, A. [Santa Cruz Institute for Particle Physics and Department of Physics, University of California, Santa Cruz, CA 95064 (United States); Bradbury, S. M. [School of Physics and Astronomy, University of Leeds, Leeds, LS2 9JT (United Kingdom); Byrum, K. [Argonne National Laboratory, 9700 S. Cass Avenue, Argonne, IL 60439 (United States); Cesarini, A.; Connolly, M. P. [School of Physics, National University of Ireland Galway, University Road, Galway (Ireland); Ciupik, L. [Astronomy Department, Adler Planetarium and Astronomy Museum, Chicago, IL 60605 (United States); Cui, W. [Department of Physics, Purdue University, West Lafayette, IN 47907 (United States); Duke, C., E-mail: amandajw@iastate.edu [Department of Physics, Grinnell College, Grinnell, IA 50112-1690 (United States); and others

2013-06-20

We report the discovery of an unidentified, extended source of very-high-energy gamma-ray emission, VER J2019+407, within the radio shell of the supernova remnant SNR G78.2+2.1, using 21.4 hr of data taken by the VERITAS gamma-ray observatory in 2009. These data confirm the preliminary indications of gamma-ray emission previously seen in a two-year (2007-2009) blind survey of the Cygnus region by VERITAS. VER J2019+407, which is detected at a post-trials significance of 7.5 standard deviations in the 2009 data, is localized to the northwestern rim of the remnant in a region of enhanced radio and X-ray emission. It has an intrinsic extent of 0.23 Degree-Sign .23 {+-} 0. Degree-Sign 03{sub stat-0 Degree-Sign .02sys}{sup +0 Degree-Sign .04} and its spectrum is well-characterized by a differential power law (dN/dE = N{sub 0} Multiplication-Sign (E/TeV){sup -{Gamma}}) with a photon index of {Gamma} = 2.37 {+-} 0.14{sub stat} {+-} 0.20{sub sys} and a flux normalization of N{sub 0} = 1.5 {+-} 0.2{sub stat} {+-} 0.4{sub sys} Multiplication-Sign 10{sup -12} photon TeV{sup -1} cm{sup -2} s{sup -1}. This yields an integral flux of 5.2 {+-} 0.8{sub stat} {+-} 1.4{sub sys} Multiplication-Sign 10{sup -12} photon cm{sup -2} s{sup -1} above 320 GeV, corresponding to 3.7% of the Crab Nebula flux. We consider the relationship of the TeV gamma-ray emission with the GeV gamma-ray emission seen from SNR G78.2+2.1 as well as that seen from a nearby cocoon of freshly accelerated cosmic rays. Multiple scenarios are considered as possible origins for the TeV gamma-ray emission, including hadronic particle acceleration at the SNR shock.