Scanning electron microscopy, x-ray diffraction, and electron microprobe analysis of calcific deposits on intrauterine contraceptive devices

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

Khan, S.R.; Wilkinson, E.J.

Deposits found on intrauterine contraceptive devices (IUDs) were studied by scanning electron microscopy, x-ray diffraction, and energy dispersive x-ray microanalysis. All seven devices, including five plastic and two copper IUDs, were coated with a crust containing cellular, acellular, and fibrillar material. The cellular material was composed of erythrocytes, leukocytes, cells of epithelial origin, sperm, and bacteria. Some of the bacteria were filamentous, with acute-angle branching. The fibrillar material appeared to be fibrin. Most of the acellular material was amorphous; calcite was identified by x-ray diffraction, and x-ray microanalysis showed only calcium. Some of the acellular material, particularly that on themore » IUD side of the crust, was organized in spherulitic crystals and was identified as calcium phosphate by x-ray microanalysis. The crust was joined to the IUD surface by a layer of fibrillar and amorphous material. It is suggested that the initial event in the formation of calcific deposits on IUD surfaces is the deposition of an amorphous and fibrillar layer. Various types of cells present in the endometrial environment adhere to this layer and then calcify. Thus, the deposition of calcific material on the IUDs is a calcification phenomenon, not unlike the formation of plaque on teeth.« less

X-ray microanalysis of porous materials using Monte Carlo simulations.

PubMed

Poirier, Dominique; Gauvin, Raynald

2011-01-01

Quantitative X-ray microanalysis models, such as ZAF or φ(ρz) methods, are normally based on solid, flat-polished specimens. This limits their use in various domains where porous materials are studied, such as powder metallurgy, catalysts, foams, etc. Previous experimental studies have shown that an increase in porosity leads to a deficit in X-ray emission for various materials, such as graphite, Cr(2) O(3) , CuO, ZnS (Ichinokawa et al., '69), Al(2) O(3) , and Ag (Lakis et al., '92). However, the mechanisms responsible for this decrease are unclear. The porosity by itself does not explain the loss in intensity, other mechanisms have therefore been proposed, such as extra energy loss by the diffusion of electrons by surface plasmons generated at the pores-solid interfaces, surface roughness, extra charging at the pores-solid interface, or carbon diffusion in the pores. However, the exact mechanism is still unclear. In order to better understand the effects of porosity on quantitative microanalysis, a new approach using Monte Carlo simulations was developed by Gauvin (2005) using a constant pore size. In this new study, the X-ray emissions model was modified to include a random log normal distribution of pores size in the simulated materials. This article presents, after a literature review of the previous works performed about X-ray microanalysis of porous materials, some of the results obtained with Gauvin's modified model. They are then compared with experimental results. Copyright © 2011 Wiley Periodicals, Inc.

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

NASA Astrophysics Data System (ADS)

Wuhrer, R.; Moran, K.

2014-03-01

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

Focussed ion beam thin sample microanalysis using a field emission gun electron probe microanalyser

NASA Astrophysics Data System (ADS)

Kubo, Y.

2018-01-01

Field emission gun electron probe microanalysis (FEG-EPMA) in conjunction with wavelength-dispersive X-ray spectrometry using a low acceleration voltage (V acc) allows elemental analysis with sub-micrometre lateral spatial resolution (SR). However, this degree of SR does not necessarily meet the requirements associated with increasingly miniaturised devices. Another challenge related to performing FEG-EPMA with a low V acc is that the accuracy of quantitative analyses is adversely affected, primarily because low energy X-ray lines such as the L- and M-lines must be employed and due to the potential of line interference. One promising means of obtaining high SR with FEG-EPMA is to use thin samples together with high V acc values. This mini-review covers the basic principles of thin-sample FEG-EPMA and describes an application of this technique to the analysis of optical fibres. Outstanding issues related to this technique that must be addressed are also discussed, which include the potential for electron beam damage during analysis of insulating materials and the development of methods to use thin samples for quantitative analysis.

Synthesis, spectroscopic investigations (X-ray, NMR and TD-DFT), antimicrobial activity and molecular docking of 2,6-bis(hydroxy(phenyl)methyl)cyclohexanone.

PubMed

Barakat, Assem; Ghabbour, Hazem A; Al-Majid, Abdullah Mohammed; Soliman, Saied M; Ali, M; Mabkhot, Yahia Nasser; Shaik, Mohammed Rafi; Fun, Hoong-Kun

2015-07-21

The synthesis of 2,6-bis(hydroxy(phenyl)methyl)cyclohexanone 1 is described. The molecular structure of the title compound 1 was confirmed by NMR, FT-IR, MS, CHN microanalysis, and X-ray crystallography. The molecular structure was also investigated by a set of computational studies and found to be in good agreement with the experimental data obtained from the various spectrophotometric techniques. The antimicrobial activity and molecular docking of the synthesized compound was investigated.

Electron-Excited X-Ray Microanalysis at Low Beam Energy: Almost Always an Adventure!

PubMed

Newbury, Dale E; Ritchie, Nicholas W M

2016-08-01

Scanning electron microscopy with energy-dispersive spectrometry has been applied to the analysis of various materials at low-incident beam energies, E 0≤5 keV, using peak fitting and following the measured standards/matrix corrections protocol embedded in the National Institute of Standards and Technology Desktop Spectrum Analyzer-II analytical software engine. Low beam energy analysis provides improved spatial resolution laterally and in-depth. The lower beam energy restricts the atomic shells that can be ionized, reducing the number of X-ray peak families available to the analyst. At E 0=5 keV, all elements of the periodic table except H and He can be measured. As the beam energy is reduced below 5 keV, elements become inaccessible due to lack of excitation of useful characteristic X-ray peaks. The shallow sampling depth of low beam energy microanalysis makes the technique more sensitive to surface compositional modification due to formation of oxides and other reaction layers. Accurate and precise analysis is possible with the use of appropriate standards and by accumulating high count spectra of unknowns and standards (>1 million counts integrated from 0.1 keV to E 0).

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

PubMed

Hunsche, Mauricio; Noga, Georg

2009-12-01

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

Characterizing individual particles on tree leaves using computer automated scanning electron microscopy

Treesearch

D. L. Johnson; D. J. Nowak; V. A. Jouraeva

1999-01-01

Leaves from twenty-three deciduous tree species and five conifer species were collected within a limited geographic range (1 km radius) and evaluated for possible application of scanning electron microscopy and X-ray microanalysis techniques of individual particle analysis (IPA). The goal was to identify tree species with leaves suitable for the automated...

Measurement of Total Calcium in Neurons by Electron Probe X-ray Microanalysis

PubMed Central

Pivovarova, Natalia B.; Andrews, S. Brian

2013-01-01

In this article the tools, techniques, and instruments appropriate for quantitative measurements of intracellular elemental content using the technique known as electron probe microanalysis (EPMA) are described. Intramitochondrial calcium is a particular focus because of the critical role that mitochondrial calcium overload plays in neurodegenerative diseases. The method is based on the analysis of X-rays generated in an electron microscope (EM) by interaction of an electron beam with the specimen. In order to maintain the native distribution of diffusible elements in electron microscopy specimens, EPMA requires "cryofixation" of tissue followed by the preparation of ultrathin cryosections. Rapid freezing of cultured cells or organotypic slice cultures is carried out by plunge freezing in liquid ethane or by slam freezing against a cold metal block, respectively. Cryosections nominally 80 nm thick are cut dry with a diamond knife at ca. -160 °C, mounted on carbon/pioloform-coated copper grids, and cryotransferred into a cryo-EM using a specialized cryospecimen holder. After visual survey and location mapping at ≤-160 °C and low electron dose, frozen-hydrated cryosections are freeze-dried at -100 °C for ~30 min. Organelle-level images of dried cryosections are recorded, also at low dose, by means of a slow-scan CCD camera and subcellular regions of interest selected for analysis. X-rays emitted from ROIs by a stationary, focused, high-intensity electron probe are collected by an energy-dispersive X-ray (EDX) spectrometer, processed by associated electronics, and presented as an X-ray spectrum, that is, a plot of X-ray intensity vs. energy. Additional software facilitates: 1) identification of elemental components by their "characteristic" peak energies and fingerprint; and 2) quantitative analysis by extraction of peak areas/background. This paper concludes with two examples that illustrate typical EPMA applications, one in which mitochondrial calcium analysis provided critical insight into mechanisms of excitotoxic injury and another that revealed the basis of ischemia resistance. PMID:24300079

Scanning electron microscopy as an analytical tool for the study of calcified intrauterine contraceptive devices

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

Khan, S.R.; Wilkinson, E.J.

Within the endometrial cavity intrauterine contraceptive devices (IUDs) become encrusted with cellular, acellular, and fibrillar substances. Scanning electron microscopy was used to study the crust. Cellular material consisted mainly of blood cells and various types of bacteria. The fibrillar material appeared to be fibrin which was omnipresent in the crust and formed a thin layer immediately over the IUD surface. X-ray microanalysis of the acellular component of the crust revealed the presence of calcium. No other major peaks were identified. Near the IUD surface characteristic calcium phosphate crystals were present. Their microanalysis showed peaks for calcium and phosphorus. X-ray diffractionmore » of the crust however, showed it to contain only calcite. It is through the use of scanning electron microscopy that calcium phosphate has been detected in the IUD crust and a fibrillar layer has been visualized on the IUD surface. This study further demonstrates the effectiveness of SEM analytical techniques in the area of biomedical research.« less

Composition, speciation and distribution of iron minerals in Imperata cylindrica.

PubMed

Amils, Ricardo; de la Fuente, Vicenta; Rodríguez, Nuria; Zuluaga, Javier; Menéndez, Nieves; Tornero, Jesús

2007-05-01

A comparative study of the roots, rhizomes and leaves of an iron hyperaccumulator plant, Imperata cylindrica, isolated from the banks of an extreme acidic environment, using complementary techniques: Mösbauer spectroscopy (MS), X-ray diffraction (XRD), scanning electron microscopy (SEM) coupled to energy-dispersive X-ray microanalysis (EDAX) and transmission electron microscopy (TEM), has shown that two main biominerals, jarosite and ferrihydrate-ferritin, accumulate in the different tissues. Jarosite accumulates mainly in roots and rhizomes, while ferritin has been detected in all the structures. A model of iron management in I. cylindrica is presented.

Effect of PbO on optical properties of tellurite glass

NASA Astrophysics Data System (ADS)

Elazoumi, S. H.; Sidek, H. A. A.; Rammah, Y. S.; El-Mallawany, R.; Halimah, M. K.; Matori, K. A.; Zaid, M. H. M.

2018-03-01

Binary (1 - x)(TeO2) - x(PbO), x = 0, 0.10, 0.15, 0.20, 0.25, 0.30 mol% glass system was fabricated using melt quenching method. X-ray diffraction (XRD) technique was employed to confirm the amorphous nature. The microanalysis of the major components was performed using energy dispersive EDX and X-ray spectrometry. Both the molar volume and the density were measured. FTIR and UV spectra were recorded at 400-4000 cm-1 and 220-800 nm, respectively. The optical band gap (Eopt), Urbach's energy (Eu), index of refraction (n) were calculated using absorption spectrum fitting (ASF) and derivation of absorption spectrum fitting (DASF) methods. Molar refraction Rm and molecular polarizability αm have been calculated according to (ASF) method.

Calcium measurements with electron probe X-ray and electron energy loss analysis.

PubMed

LeFurgey, A; Ingram, P

1990-03-01

This paper presents a broad survey of the rationale for electron probe X-ray microanalysis (EPXMA) and the various methods for obtaining qualitative and quantitative information on the distribution and amount of elements, particularly calcium, in cryopreserved cells and tissues. Essential in an introductory consideration of microanalysis in biological cryosections is the physical basis for the instrumentation, fundamentals of X-ray spectrometry, and various analytical modes such as static probing and X-ray imaging. Some common artifacts are beam damage and contamination. Inherent pitfalls of energy dispersive X-ray systems include Si escape peaks, doublets, background, and detector calibration shifts. Quantitative calcium analysis of thin cryosections is carried out in real time using a multiple least squares fitting program on filtered X-ray spectra and normalizing the calcium peak to a portion of the continuum. Recent work includes the development of an X-ray imaging system where quantitative data can be retrieved off-line. The minimum detectable concentration of calcium in biological cryosections is approximately 300 mumole kg dry weight with a spatial resolution of approximately 100 A. The application of electron energy loss (EELS) techniques to the detection of calcium offers the potential for greater sensitivity and spatial resolution in measurement and imaging. Determination of mass thickness with EELS can facilitate accurate calculation of wet weight concentrations from frozen hydrated and freeze-dried specimens. Calcium has multiple effects on cell metabolism, membrane transport and permeability and, thus, on overall cell physiology or pathophysiology. Cells can be rapidly frozen for EPXMA during basal or altered functional conditions to delineate the location and amount of calcium within cells and the changes in location and concentration of cations or anions accompanying calcium redistribution. Recent experiments in our laboratory document that EPXMA in combination with other biochemical and electrophysiological techniques can be used to study, for example, sodium and calcium compartmentation in cultured cardiac cells. Such analyses can also be used to clarify the role of calcium in anoxic renal cell injury and to evaluate proposed ionic defects in cells of individuals with cystic fibrosis.

Single-particle mineralogy of Chinese soil particles by the combined use of low-Z particle electron probe X-ray microanalysis and attenuated total reflectance-FT-IR imaging techniques.

PubMed

Malek, Md Abdul; Kim, Bowha; Jung, Hae-Jin; Song, Young-Chul; Ro, Chul-Un

2011-10-15

Our previous work on the speciation of individual mineral particles of micrometer size by the combined use of attenuated total reflectance FT-IR (ATR-FT-IR) imaging and a quantitative energy-dispersive electron probe X-ray microanalysis technique (EPMA), low-Z particle EPMA, demonstrated that the combined use of these two techniques is a powerful approach for looking at the single-particle mineralogy of externally heterogeneous minerals. In this work, this analytical methodology was applied to characterize six soil samples collected at arid areas in China, in order to identify mineral types present in the samples. The six soil samples were collected from two types of soil, i.e., loess and desert soils, for which overall 665 particles were analyzed on a single particle basis. The six soil samples have different mineralogical characteristics, which were clearly differentiated in this work. As this analytical methodology provides complementary information, the ATR-FT-IR imaging on mineral types, and low-Z particle EPMA on the morphology and elemental concentrations, on the same individual particles, more detailed information can be obtained using this approach than when either low-Z particle EPMA or ATR-FT-IR imaging techniques are used alone, which has a great potential for the characterization of Asian dust and mineral dust particles. © 2011 American Chemical Society

An expert system for chemical speciation of individual particles using low-Z particle electron probe X-ray microanalysis data.

PubMed

Ro, Chul-Un; Kim, HyeKyeong; Van Grieken, René

2004-03-01

An electron probe X-ray microanalysis (EPMA) technique, using an energy-dispersive X-ray detector with an ultrathin window, designated a low-Z particle EPMA, has been developed. The low-Z particle EPMA allows the quantitative determination of concentrations of low-Z elements, such as C, N, and O, as well as chemical elements that can be analyzed by conventional energy-dispersive EPMA, in individual particles. Since a data set is usually composed of data for several thousands of particles in order to make environmentally meaningful observations of real atmospheric aerosol samples, the development of a method that fully extracts chemical information contained in the low-Z particle EPMA data is important. An expert system that can rapidly and reliably perform chemical speciation from the low-Z particle EPMA data is presented. This expert system tries to mimic the logic used by experts and is implemented by applying macroprogramming available in MS Excel software. Its feasibility is confirmed by applying the expert system to data for various types of standard particles and a real atmospheric aerosol sample. By applying the expert system, the time necessary for chemical speciation becomes shortened very much and detailed information on particle data can be saved and extracted later if more information is needed for further analysis.

Emerging surface characterization techniques for carbon steel corrosion: a critical brief review.

PubMed

Dwivedi, D; Lepkova, K; Becker, T

2017-03-01

Carbon steel is a preferred construction material in many industrial and domestic applications, including oil and gas pipelines, where corrosion mitigation using film-forming corrosion inhibitor formulations is a widely accepted method. This review identifies surface analytical techniques that are considered suitable for analysis of thin films at metallic substrates, but are yet to be applied to analysis of carbon steel surfaces in corrosive media or treated with corrosion inhibitors. The reviewed methods include time of flight-secondary ion mass spectrometry, X-ray absorption spectroscopy methods, particle-induced X-ray emission, Rutherford backscatter spectroscopy, Auger electron spectroscopy, electron probe microanalysis, near-edge X-ray absorption fine structure spectroscopy, X-ray photoemission electron microscopy, low-energy electron diffraction, small-angle neutron scattering and neutron reflectometry, and conversion electron Moessbauer spectrometry. Advantages and limitations of the analytical methods in thin-film surface investigations are discussed. Technical parameters of nominated analytical methods are provided to assist in the selection of suitable methods for analysis of metallic substrates deposited with surface films. The challenges associated with the applications of the emerging analytical methods in corrosion science are also addressed.

Emerging surface characterization techniques for carbon steel corrosion: a critical brief review

NASA Astrophysics Data System (ADS)

Dwivedi, D.; Lepkova, K.; Becker, T.

2017-03-01

Carbon steel is a preferred construction material in many industrial and domestic applications, including oil and gas pipelines, where corrosion mitigation using film-forming corrosion inhibitor formulations is a widely accepted method. This review identifies surface analytical techniques that are considered suitable for analysis of thin films at metallic substrates, but are yet to be applied to analysis of carbon steel surfaces in corrosive media or treated with corrosion inhibitors. The reviewed methods include time of flight-secondary ion mass spectrometry, X-ray absorption spectroscopy methods, particle-induced X-ray emission, Rutherford backscatter spectroscopy, Auger electron spectroscopy, electron probe microanalysis, near-edge X-ray absorption fine structure spectroscopy, X-ray photoemission electron microscopy, low-energy electron diffraction, small-angle neutron scattering and neutron reflectometry, and conversion electron Moessbauer spectrometry. Advantages and limitations of the analytical methods in thin-film surface investigations are discussed. Technical parameters of nominated analytical methods are provided to assist in the selection of suitable methods for analysis of metallic substrates deposited with surface films. The challenges associated with the applications of the emerging analytical methods in corrosion science are also addressed.

Emerging surface characterization techniques for carbon steel corrosion: a critical brief review

PubMed Central

Dwivedi, D.; Becker, T.

2017-01-01

Carbon steel is a preferred construction material in many industrial and domestic applications, including oil and gas pipelines, where corrosion mitigation using film-forming corrosion inhibitor formulations is a widely accepted method. This review identifies surface analytical techniques that are considered suitable for analysis of thin films at metallic substrates, but are yet to be applied to analysis of carbon steel surfaces in corrosive media or treated with corrosion inhibitors. The reviewed methods include time of flight-secondary ion mass spectrometry, X-ray absorption spectroscopy methods, particle-induced X-ray emission, Rutherford backscatter spectroscopy, Auger electron spectroscopy, electron probe microanalysis, near-edge X-ray absorption fine structure spectroscopy, X-ray photoemission electron microscopy, low-energy electron diffraction, small-angle neutron scattering and neutron reflectometry, and conversion electron Moessbauer spectrometry. Advantages and limitations of the analytical methods in thin-film surface investigations are discussed. Technical parameters of nominated analytical methods are provided to assist in the selection of suitable methods for analysis of metallic substrates deposited with surface films. The challenges associated with the applications of the emerging analytical methods in corrosion science are also addressed. PMID:28413351

Effect of shape and thickness of asbestos bundles and fibres on EDS microanalysis: A Monte Carlo simulation

NASA Astrophysics Data System (ADS)

Moro, D.; Valdre, G.

2016-02-01

Quantitative microanalysis of tiny asbestos mineral fibres by scanning electron microscopy equipped with energy-dispersive X-ray spectroscopy (SEM-EDS) still represents a complex analytical issue. This complexity arises from the variable fibre shape and small thickness (< 5 μm) compared with the penetration of the incident electron beam. Here, we present the results of Monte Carlo simulations of chrysotile, crocidolite and amosite fibres (and bundles of fibres) of circular and square section and thicknesses from 0.1 μm to 10 μm, to investigate the effect of shape and thickness on SEM-EDS microanalysis. The influence of shape and thickness on the simulated spectrum was investigated for electron beam energies of 5, 15 and 25 keV, respectively. A strong influence of the asbestos bundles and fibres shape and thickness on the detected EDS X-ray intensity was observed. The X-ray intensity trends as a function of fibre thickness showed a non-linear dependence for all the elements and minerals. In general, the X-ray intensities showed a considerable reduction for thicknesses below about 5 μm at 5 keV, 2 μm at 15 keV, and 5 μm at 25 keV. Correction parameters, k-ratios, for the asbestos fibre thickness effect, are reported.

Chemical speciation of individual airborne particles by the combined use of quantitative energy-dispersive electron probe X-ray microanalysis and attenuated total reflection Fourier transform-infrared imaging techniques.

PubMed

Song, Young-Chul; Ryu, JiYeon; Malek, Md Abdul; Jung, Hae-Jin; Ro, Chul-Un

2010-10-01

In our previous work, it was demonstrated that the combined use of attenuated total reflectance (ATR) FT-IR imaging and quantitative energy-dispersive electron probe X-ray microanalysis (ED-EPMA), named low-Z particle EPMA, had the potential for characterization of individual aerosol particles. Additionally, the speciation of individual mineral particles was performed on a single particle level by the combined use of the two techniques, demonstrating that simultaneous use of the two single particle analytical techniques is powerful for the detailed characterization of externally heterogeneous mineral particle samples and has great potential for characterization of atmospheric mineral dust aerosols. These single particle analytical techniques provide complementary information on the physicochemical characteristics of the same individual particles, such as low-Z particle EPMA on morphology and elemental concentrations and the ATR-FT-IR imaging on molecular species, crystal structures, functional groups, and physical states. In this work, this analytical methodology was applied to characterize an atmospheric aerosol sample collected in Incheon, Korea. Overall, 118 individual particles were observed to be primarily NaNO(3)-containing, Ca- and/or Mg-containing, silicate, and carbonaceous particles, although internal mixing states of the individual particles proved complicated. This work demonstrates that more detailed physiochemical properties of individual airborne particles can be obtained using this approach than when either the low-Z particle EPMA or ATR-FT-IR imaging technique is used alone.

The Effect of the Acetone Extract of Arctotis arctotoides (Asteraceae) on the Growth and Ultrastructure of Some Opportunistic Fungi Associated with HIV/AIDS

PubMed Central

Otang, Wilfred M.; Grierson, Donald S.; Ndip, Roland N.

2011-01-01

In this study, the effect of the acetone extract of Arctotis arctotoides (L.f.) O. Hoffm. (Asteraceae) on the growth and ultrastructure of some opportunistic fungi associated with HIV/AIDS was analyzed by means of scanning electron microscope (SEM). Remarkable morphological alterations in the fungal mycelia which were attributed to the loss of cell wall strength ranged from loss of turgidity and uniformity, collapse of entire hyphae to evident destruction of the hyphae. The elements responsible for giving the fungi their characteristic virulence were detected and quantified by energy dispersive X-ray microanalysis techniques. X-ray microanalysis showed the specific spectra of sodium, potassium and sulfur as the principal intersection of the four pathogenic fungi studied. Since these ions have the potential of fostering fungal invasion by altering the permeability of hosts’ membranes, their presence was considered inherent to the pathogenicity of the opportunistic fungi. Hence, these findings indicate the potential of the crude extract of A. arctotoides in preventing fungal invasion and subsequent infection of host’s membranes. PMID:22272130

Relative intranuclear magnesium and phosphorus contents in normal and tumor cells of the human thyroid gland as revealed by energy-dispersive X-ray microanalysis.

PubMed

Lukács, G L; Zs-Nagy, I; Steiber, J; Györi, F; Balázs, G

1996-01-01

Energy dispersive X-ray microanalysis was performed on altogether 42 surgically removed tissue specimens of 32 patients, which were taken either from intact thyroid parts or various histopathologically verified tumors of the thyroid gland. The tissue specimens were processed with the freeze-fracture-freeze-drying technique and then analyzed in the so-called bulk specimen form. The studies were carried out during the years 1980-81, when intranuclear monovalent ionic composition was studied in detail. From the retained total elemental peak list, it was possible to calculate retrospectively the relative intranuclear Mg and P contents. The data processed by nested (hierarchical) analysis of variance show that the intranuclear Mg content of the 5 diagnostic groups (normal thyroid tissue, thyroiditis, benign adenomas, differentiated carcinomas and undifferentiated thyroid tumors) increases significantly, in parallel with the increasing malignancy, but the P content remains unchanged. One can conclude that the elevated intranuclear Mg content in the tumors of high malignancy may be of diagnostic importance, and a warning signal for the therapeutic approaches based on Mg-supplementations.

An indirect method for quantitation of cellular zinc content of Timm-stained cerebellar samples by energy dispersive X-ray microanalysis.

PubMed

Farkas, I; Szerdahelyi, P; Kása, P

1988-01-01

The absolute concentration of zinc in the Purkinje cells of the rat cerebellum was determined by means of energy dispersive X-ray microanalysis (EDAX). Gelatine blocks with known zinc concentrations were stained by Timm's sulphide-silver method, and their silver concentrations were measured by EDAX. A linear correlation was found between the zinc and silver concentrations and this linear function was used as a quantitative calibration for evaluation of sulphide-silver staining, after perfusion with sodium-sulphide solution, fixation with glutaraldehyde, cryostat sectioning and staining of cerebellar samples in Timm's reagent.

Environmental Remediation Science at Beamline X26A at the National Synchrotron Light Source- Final Report

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

Bertsch, Paul

2013-11-07

The goal of this project was to provide support for an advanced X-ray microspectroscopy facility at the National Synchrotron Light Source, Brookhaven National Laboratory. This facility is operated by the University of Chicago and the University of Kentucky. The facility is available to researchers at both institutions as well as researchers around the globe through the general user program. This facility was successfully supported during the project period. It provided access to advanced X-ray microanalysis techniques which lead to fundamental advances in understanding the behavior of contaminants and geochemistry that is applicable to environmental remediation of DOE legacy sites asmore » well as contaminated sites around the United States and beyond.« less

Electron microscopy methods in studies of cultural heritage sites

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

Vasiliev, A. L., E-mail: a.vasiliev56@gmail.com; Kovalchuk, M. V.; Yatsishina, E. B.

The history of the development and application of scanning electron microscopy (SEM), transmission electron microscopy (TEM), and energy-dispersive X-ray microanalysis (EDXMA) in studies of cultural heritage sites is considered. In fact, investigations based on these methods began when electron microscopes became a commercial product. Currently, these methods, being developed and improved, help solve many historical enigmas. To date, electron microscopy combined with microanalysis makes it possible to investigate any object, from parchment and wooden articles to pigments, tools, and objects of art. Studies by these methods have revealed that some articles were made by ancient masters using ancient “nanotechnologies”; hence,more » their comprehensive analysis calls for the latest achievements in the corresponding instrumental methods and sample preparation techniques.« less

Electron microscopy methods in studies of cultural heritage sites

NASA Astrophysics Data System (ADS)

Vasiliev, A. L.; Kovalchuk, M. V.; Yatsishina, E. B.

2016-11-01

The history of the development and application of scanning electron microscopy (SEM), transmission electron microscopy (TEM), and energy-dispersive X-ray microanalysis (EDXMA) in studies of cultural heritage sites is considered. In fact, investigations based on these methods began when electron microscopes became a commercial product. Currently, these methods, being developed and improved, help solve many historical enigmas. To date, electron microscopy combined with microanalysis makes it possible to investigate any object, from parchment and wooden articles to pigments, tools, and objects of art. Studies by these methods have revealed that some articles were made by ancient masters using ancient "nanotechnologies"; hence, their comprehensive analysis calls for the latest achievements in the corresponding instrumental methods and sample preparation techniques.

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

PubMed

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

2018-06-24

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

Microanalysis of iron oxidation state in iron oxides using X Ray Absorption Near Edge Structure (XANES)

NASA Technical Reports Server (NTRS)

Sutton, S. R.; Delaney, J.; Bajt, S.; Rivers, M. L.; Smith, J. V.

1993-01-01

An exploratory application of x ray absorption near edge structure (XANES) analysis using the synchrotron x ray microprobe was undertaken to obtain Fe XANES spectra on individual sub-millimeter grains in conventional polished sections. The experiments concentrated on determinations of Fe valence in a suite of iron oxide minerals for which independent estimates of the iron speciation could be made by electron microprobe analysis and x ray diffraction.

Ultrastructural and x-ray microanalytical observations of minocycline-related hyperpigmentation of the skin

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

Sato, S.; Murphy, G.F.; Bernhard, J.D.

1981-09-01

In order to elucidate the nature and distribution of the pigment responsible for the circumscribed blue-black cutaneous hyperpigmentation occurring after administration of minocycline hydrochloride, transmission electron microscopy and energy-dispersive electron x-ray microanalysis were performed on lesional skin. Ultrastructural observations demonstrated electron-dense iron-containing particles either incorporated into a variety of siderosomes, within dermal histiocytes, free within the cytoplasm, or, rarely, scattered among dermal collagen fibers. Electron x-ray microanalysis confirmed iron content present within these particles. Although siderosomal inclusions contained occasional melanosome complexes, the degree of deposition of electron-dense iron-containing particles in dermal histiocytes seemed to be primarily responsible for the blue-blackmore » discoloration of the skin. The present study is an investigation of the structure and composition of the pigment responsible for minocycline-related cutaneous hyperpigmentation.« less

Scattered electrons in microscopy and microanalysis

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

Ottensmeyer, F.P.

The use of scattered electrons alone for direct imaging of biological specimens makes it possible to obtain structural information at atomic and near-atomic spatial resolutions of 0.3 to 0.5 nanometer. While this is not as good as the resolution possible with x-ray crystallography, such an approach provides structural information rapidly on individual macromolecules that have not been, and possibly cannot be, crystallized. Analysis of the spectrum of energies of scattered electrons and imaging of the latter with characteristic energy bands within the spectrum produces a powerful new technique of atomic microanalysis. This technique, which has a spatial resolution of aboutmore » 0.5 nanometer and a minimum detection sensitivity of about 50 atoms of phosphorus, is especially useful for light atom analysis and appears to have applications in molecular biology, cell biology, histology, pathology, botany, and many other fields.« less

Scattered electrons in microscopy and microanalysis

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

Ottensmeyer, F.P.

The use of scattered electrons alone for direct imaging of biological specimens makes it possible to obtain structural information at atomic and near-atomic spatial resolutions of 0.3 to 0.5 nanometer. While this is not as good as the resolution possible with x-ray crystallography, such an approach provides structural information rapidly on individual macromolecules that have not been, and possibly cannot be, crystallized. Analysis of the spectrum of energies of scattered electrons and imaging of the latter with characteristic energy bands within the spectrum produce a powerful new technique of atomic microanalysis. This technique, which has a spatial resolution of aboutmore » 0.5 nanometer and a minimum detection sensitivity of about 50 atoms of phosphorus, is especially useful for light atom analysis and appears to have applications in molecular biology, cell biology, histology, pathology, botany, and many other fields.« less

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

NASA Technical Reports Server (NTRS)

Carpenter, P. K.

2005-01-01

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

Microbeam X-ray analysis in Poland - past and future

NASA Astrophysics Data System (ADS)

Kusinski, J.

2010-02-01

The article provides an overview of the development of electron beam X-ray microanalysis (EPMA) in Poland. Since the introduction by Prof. Bojarski of EMPA over 45 years ago, tremendous advances in methodologies and in instrumentation have been made in order to improve the precision of quantitative compositional analysis, spatial resolution and analytical sensitivity. This was possible due to the activity of Applied Crystallography Committee at the Polish Academy of Sciences, as well as the groups of researches working in the Institute for Ferrous Metallurgy (Gliwice), the Technical University of Warsaw, the Silesian Technical University (Katowice), the AGH-University of Sciences and Technology (Krakow), and the Institute of Materials Science and Metallurgy Polish Academy of Sciences (Krakow). Based on the research examples realized by these teams, conferences, seminars and congresses organized, as well as books and academic textbooks issued, the evolution of electron beam X-ray microanalysis in Poland is demonstrated.

The X-ray Fluorescence Microscopy Beamline at the Australian Synchrotron

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

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

2011-09-09

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

Single-particle characterization of urban aerosol particles collected in three Korean cites using low-Z electron probe X-ray microanalysis.

PubMed

Ro, Chul-Un; Kim, HyeKyeong; Oh, Keun-Young; Yea, Sun Kyung; Lee, Chong Bum; Jang, Meongdo; Van Grieken, René

2002-11-15

A recently developed single-particle analytical technique, called low-Z electron probe X-ray microanalysis (low-Z EPMA), was applied to characterize urban aerosol particles collected in three cities of Korea (Seoul, CheongJu, and ChunCheon) on single days in the winter of 1999. In this study, it is clearly demonstrated that the low-Z EPMA technique can provide detailed and quantitative information on the chemical composition of particles in the urban atmosphere. The collected aerosol particles were analyzed and classified on the basis of their chemical species. Various types of particles were identified, such as soil-derived, carbonaceous, marine-originated, and anthropogenic particles. In the sample collected in Seoul, carbonaceous, aluminosilicates, silicon dioxide, and calcium carbonate aerosol particles were abundantly encountered. In the CheongJu and ChunCheon samples, carbonaceous, aluminosilicates, reacted sea salts, and ammonium sulfate aerosol particles were often seen. However, in the CheongJu sample, ammonium sulfate particles were the most abundant in the fine fraction. Also, calcium sulfate and nitrate particles were significantly observed. In the ChunCheon sample, organic particles were the most abundant in the fine fraction. Also, sodium nitrate particles were seen at high levels. The ChunCheon sample seemed to be strongly influenced by sea-salt aerosols originating from the Yellow Sea, which is located about 115 km away from the city.

Rigorous quantitative elemental microanalysis by scanning electron microscopy/energy dispersive x-ray spectrometry (SEM/EDS) with spectrum processing by NIST DTSA-II

NASA Astrophysics Data System (ADS)

Newbury, Dale E.; Ritchie, Nicholas W. M.

2014-09-01

Quantitative electron-excited x-ray microanalysis by scanning electron microscopy/silicon drift detector energy dispersive x-ray spectrometry (SEM/SDD-EDS) is capable of achieving high accuracy and high precision equivalent to that of the high spectral resolution wavelength dispersive x-ray spectrometer even when severe peak interference occurs. The throughput of the SDD-EDS enables high count spectra to be measured that are stable in calibration and resolution (peak shape) across the full deadtime range. With this high spectral stability, multiple linear least squares peak fitting is successful for separating overlapping peaks and spectral background. Careful specimen preparation is necessary to remove topography on unknowns and standards. The standards-based matrix correction procedure embedded in the NIST DTSA-II software engine returns quantitative results supported by a complete error budget, including estimates of the uncertainties from measurement statistics and from the physical basis of the matrix corrections. NIST DTSA-II is available free for Java-platforms at: http://www.cstl.nist.gov/div837/837.02/epq/dtsa2/index.html).

Evaluation of bone response to titanium-coated polymethyl methacrylate resin (PMMA) implants by X-ray tomography.

PubMed

Shalabi, Manal M; Wolke, Johannes G C; Cuijpers, Vincent M J I; Jansen, John A

2007-10-01

High-resolution three-dimensional data about the bone response to oral implants can be obtained by using microfocus computer tomography. However, a disadvantage is that metallic implants cause streaking artifacts due to scattering of X-rays, which prevents an accurate evaluation of the interfacial bone-to-implant contact. It has been suggested that the use of thin titanium coatings deposited on polymeric implants can offer an alternative option for analyzing bone contact using micro-CT imaging. Consequently, the aim of the current study was to investigate bone behavior to titanium-coated polymethylmethacrylate (PMMA) implants by micro-CT and histological evaluation. For the experiment titanium-coated PMMA implants were used. The implants had a machined threaded appearance and were provided with a 400-500 nm thick titanium coating. The implants were inserted in the right or left tibia of 10 goats. After an implantation period of 12 weeks the implants were retrieved and prepared for micro-computer tomography (microCT), light microscopy, and X-ray microanalysis. The micro-CT showed that the screw-threads and typical implant configuration were well maintained through the installation procedure. Overall, histological responses showed that the titanium-coated implants were well tolerated and caused no atypical tissue response. In addition, the bone was seen in direct contact with the titanium-coated layer. The X-ray microanalysis results confirmed the light microscopical data. In conclusion, the obtained results proof the final use of titanium-coated PMMA implants for evaluation of the bone-implant response using microCT. However, this study also confirms that for a proper analysis of the bone-implant interface the additional use of microscopical techniques is still required.

Calcium transport mechanism in molting crayfish revealed by microanalysis

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

Mizuhira, V.; Ueno, M.

1983-01-01

Crayfish provide a good model in which to study the transport mechanism of Ca ions. During the molting stage, decalcified Ca ions are transferred into the blood and accumulate in the gastrolith epithelium, after which a gastrolith is formed on the surface of the epithelium. The gastrolith is dissolved in the stomach after molting, and the Ca is reabsorbed and redistributed throughout the newly formed exoskeleton. We studied the mechanism of Ca transport by cytochemical precipitation of Ca ions and by electron microanalysis, including X-ray microanalysis (EDX) and electron energy-loss spectroscopy (EELS), with a computer. In EDX analysis, the finemore » precipitates of K-antimonate in the gastrolith mitochondria clearly defined Ca with antimony; we also observed a large amount of Ca-oxalate in the mitochondria, and Ca-K X-ray pulses were clearly defined. Ca-K X-rays were also detected from fresh freeze-substituted mitochondria. Finally, we succeeded in taking a Ca-L EELS image from the mitochondria of fresh freeze-substituted thin sections. Only a very small amount of Ca was detected from the cell membrane and other organelles. Ca-adenosine triphosphatase (ATPase) and Mg-ATPase activity was also very clearly demonstrated in the mitochondria. These enzymes may play an important role in Ca metabolism.« less

High-resolution x-ray imaging for microbiology at the Advanced Photon Source

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

Lai, B.; Kemner, K. M.; Maser, J.

1999-11-02

Exciting new applications of high-resolution x-ray imaging have emerged recently due to major advances in high-brilliance synchrotrons sources and high-performance zone plate optics. Imaging with submicron resolution is now routine with hard x-rays: the authors have demonstrated 150 run in the 6--10 keV range with x-ray microscopes at the Advanced Photon Source (APS), a third-generation synchrotrons radiation facility. This has fueled interest in using x-ray imaging in applications ranging from the biomedical, environmental, and materials science fields to the microelectronics industry. One important application they have pursued at the APS is a study of the microbiology of bacteria and theirmore » associated extracellular material (biofilms) using fluorescence microanalysis. No microscopy techniques were previously available with sufficient resolution to study live bacteria ({approx}1 {micro}m x 4 {micro}m in size) and biofilms in their natural hydrated state with better than part-per-million elemental sensitivity and the capability of determining g chemical speciation. In vivo x-ray imaging minimizes artifacts due to sample fixation, drying, and staining. This provides key insights into the transport of metal contaminants by bacteria in the environment and potential new designs for remediation and sequestration strategies.« less

Normal incidence X-ray mirror for chemical microanalysis

DOEpatents

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

1990-01-01

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

Australian Red Dune Sand: A Potential Martian Regolith Analog

NASA Technical Reports Server (NTRS)

Kuhlman, K. R.; Marshall, J.; Evans, N. D.; Luttge, A.

2001-01-01

To demonstrate the potential scientific and technical merits of in situ microscopy on Mars, we analyzed a possible Martian regolith analog - an acolian red dune sand from the central Australian desert (near Mt. Olga). This sand was chosen for its ubiquitous red coating and the desert environment in which is it found. Grains of this sand were analyzed using a variety of microanalytical techniques. A database of detailed studies of such terrestrial analogs would assist the study of geological and astrobiological specimens in future missions to Mars. Potential instrument concepts for in situ deployment on Mars include local electrode atom probe nanoanalysis (LEAP), vertical scanning white light interferometry (VSWLI), scanning electron microscopies, energy dispersive x-ray microanalysis (EDX), atomic force microscopy (AFM) and X-ray diffraction (XRD). While in situ deployment of these techniques is many years away, ground-based studies using these analytical techniques extend our understanding of the data obtained from instruments to be flown in the near future.

Advances toward submicron resolution optics for x-ray instrumentation and applications

NASA Astrophysics Data System (ADS)

Cordier, Mark; Stripe, Benjamin; Yun, Wenbing; Lau, S. H.; Lyon, Alan; Reynolds, David; Lewis, Sylvia J. Y.; Chen, Sharon; Semenov, Vladimir A.; Spink, Richard I.; Seshadri, Srivatsan

2017-08-01

Sigray's axially symmetric x-ray optics enable advanced microanalytical capabilities for focusing x-rays to microns-scale to submicron spot sizes, which can potentially unlock many avenues for laboratory micro-analysis. The design of these optics allows submicron spot sizes even at low x-ray energies, enabling research into low atomic number elements and allows increased sensitivity of grazing incidence measurements and surface analysis. We will discuss advances made in the fabrication of these double paraboloidal mirror lenses designed for use in laboratory x-ray applications. We will additionally present results from as-built paraboloids, including surface figure error and focal spot size achieved to-date.

X-ray microanalysis of the fingernails in term and preterm infants

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

Sirota, L.; Straussberg, R.; Fishman, P.

1988-08-01

The element content of the fingernails of 10 term and 14 preterm infants, clipped for the first time after delivery, was determined by x-ray microanalysis. The results showed a decrease in sulfur and aluminum, and a higher chlorine content in term infants in comparison with preterm ones, the difference being statistically significant. Sodium, potassium, calcium, and zinc content did not differ in the two groups. Copper, iron, magnesium, aluminum, and phosphorus were detected in trace amounts only. Cobalt was not detected in the fingernails of newborns in either group. The elevated content of aluminum in the fingernails of preterm infantsmore » may be a clue to the osteopenia observed in these infants.« less

Archaeometric study of black-coated pottery from Pompeii by different analytical techniques.

PubMed

Scarpelli, Roberta; Clark, Robin J H; De Francesco, Anna Maria

2014-01-01

Complementary spectroscopic methods were used to characterize ceramic body and black coating of fine pottery found at Pompeii (Italy). This has enabled us to investigate local productions and to clarify the technological changes over the 4th-1st centuries BC. Two different groups of ceramics were originally distinguished on the basis of macroscopic observations. Optical microscopy (OM), X-ray diffraction (XRD) and X-ray fluorescence (XRF) seem to indicate the usage of the same raw materials for the production of black-coated ceramics at Pompeii for about three centuries. Raman microscopy (RM) and micro-analysis (SEM/EDS) suggest different production treatments for both raw material processing and firing practice (duration of the reducing step and the cooling rate). Copyright © 2013 Elsevier B.V. All rights reserved.

High Rate Deposition of Thick CrN and Cr2N Coatings Using Modulated Pulse Power (MPP) Magnetron Sputtering

DTIC Science & Technology

2010-12-01

in the conventional Bragg-Bentano mode. The residual stress of the coatings was measured by glancing incident angle XRD (GIXRD) in the same X - ray ...micro-analysis (EPMA), x - ray diffraction (XRD), field-emission scanning electron microscopy (FESEM), nanoindentation, scratch test, and ball-on...the coatings was determined by XRD using a SIEMENS X - ray diffractometer (Model KRISTALLOFLEX-810) operated with K-alpha Cu radiation (30 kV and 20 mA

Application of electron probe X-ray microanalysis to calcification studies of bone and cartilage.

PubMed

Landis, W J

1979-01-01

The use of electron probe x-ray microanalysis in previous studies of bone and cartilage has been reviewed with emphasis on the results which have contributed to some of the current concepts of the mechanism of mineralization in these tissues. A number of investigations continuing in the author's laboratory utilizing high spatial resolution x-ray microanalysis and anhydrous methods of specimen preparation are described, including aspects concerning the derivation of calibration curves from synthetic calcium phosphate solids, qualitative and quantitative analyses of calcium and phosphorus in bone from embryonic chicks and in growth plate cartilage from rats, and the role of organically-bound phosphorus in mineralizing tissues. The data obtained have helped identify brushite, CaHPO4-2H2O, as the major crystalline solid phase of calcium phosphate in the earliest mineral deposits of bone tissue, brushite and poorly crystalline hydroxyapatite in bone mineral of increasing age, and poorly crystalline hydroxyapatite in the most mature mineral portions of the tissue. Growth plate cartilage examination has revealed calcium and phosphorus in single mitochondrial granules within chondrocytes and in certain extracellular particles distinct from matrix vesicles. These results have provided important information about the possible roles of cells, extracellular components, and the organic matrix in the regulation of mineralization and about the composition, structure, and organization of the mineral phase as a function of progressively increasing age and maturation of the tissues studied.

Monte Carlo Simulation to Determine Geometry Effects on Quantitative X-ray Microanalysis in Plant Cell Walls Using Gelatin Standards

NASA Astrophysics Data System (ADS)

Tylko, Grzegorz; Dubchak, Sergyi; Banach, Zuzanna; Turnau, Katarzyna

2010-04-01

Monte Carlo simulations of gelatin matrices with known elemental concentrations confirmed the suitability of protein standards to quantify elements of cellulose material in x-ray microanalysis. However, gelatin standards and cellulose plant cell walls differ in structure, what influences x-ray generation and emission in both specimens. The goal of the project was to establish the influence of gelatin structure on x-ray generation and its usefulness to calculate elemental concentrations in plant cell walls of different width. Roots of Medicago truncatula as well as gelatin standards with known elemental composition were prepared according to freeze-drying protocols. The thermanox polymer was chosen to establish background formation for flat and compact organic materials. All analyses were performed with the scanning electron microscope operated at 10 keV and probe current of 350 pA. The Monte Carlo code Casino was applied to calculate the intensities of the generated and the emitted x-rays from biological matrix of different width. No topography effects of gelatin structure were visible when the raster mode of electron impact was applied to the specimen. Monte Carlo simulations of gelatin of different width revealed that a significant decrease of the generated x-ray intensity appears at the width of the specimen around 3.5 μm. However, an increase of emission of low energy x-ray intensities (Na, Mg) was noted at 3.5 μm size with constant emission of higher energy x-rays (Cl, K) down to 2.5 μm width. It determines the minimal size of plant specimen useful for comparison to bulk gelatin standard when quantitative analysis is performed for biologically important elements.

Elemental imaging at the nanoscale: NanoSIMS and complementary techniques for element localisation in plants.

PubMed

Moore, Katie L; Lombi, Enzo; Zhao, Fang-Jie; Grovenor, Chris R M

2012-04-01

The ability to locate and quantify elemental distributions in plants is crucial to understanding plant metabolisms, the mechanisms of uptake and transport of minerals and how plants cope with toxic elements or elemental deficiencies. High-resolution secondary ion mass spectrometry (SIMS) is emerging as an important technique for the analysis of biological material at the subcellular scale. This article reviews recent work using the CAMECA NanoSIMS to determine elemental distributions in plants. The NanoSIMS is able to map elemental distributions at high resolution, down to 50 nm, and can detect very low concentrations (milligrams per kilogram) for some elements. It is also capable of mapping almost all elements in the periodic table (from hydrogen to uranium) and can distinguish between stable isotopes, which allows the design of tracer experiments. In this review, particular focus is placed upon studying the same or similar specimens with both the NanoSIMS and a wide range of complementary techniques, showing how the advantages of each technique can be combined to provide a fuller data set to address complex scientific questions. Techniques covered include optical microscopy, synchrotron techniques, including X-ray fluorescence and X-ray absorption spectroscopy, transmission electron microscopy, electron probe microanalysis, particle-induced X-ray emission and inductively coupled plasma mass spectrometry. Some of the challenges associated with sample preparation of plant material for SIMS analysis, the artefacts and limitations of the technique and future trends are also discussed.

Exceptional case of bone resorption in an osteo-odonto-keratoprosthesis. A scanning electron microscopy and X-ray microanalysis study

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

Caiazza, S.; Falcinelli, G.; Pintucci, S.

1990-01-01

This article reports the findings of investigations on an osteo-odonto-keratoprosthesis in an eye that was enucleated owing to severe complications 12 years after implantation. Scanning electron microscopy and electron probe X-ray microanalysis showed extensive resorption of the bone that was used as a supporting element in the kind of transcorneal prosthesis developed by Strampelli. The destructive process, in addition to surgical trauma, has been associated with the early and recurrent bacterial infections relating to the presence of Staphylococcus epidermidis. The need to control the occurrence of primary bacterial infections in traumatized tissues during operations as well as further infectious situations,more » given the enhanced antibiotic-resistence of bacteria, is emphasized.« less

Measurement of Trace Constituents by Electron-Excited X-Ray Microanalysis with Energy-Dispersive Spectrometry.

PubMed

Newbury, Dale E; Ritchie, Nicholas W M

2016-06-01

Electron-excited X-ray microanalysis performed with scanning electron microscopy and energy-dispersive spectrometry (EDS) has been used to measure trace elemental constituents of complex multielement materials, where "trace" refers to constituents present at concentrations below 0.01 (mass fraction). High count spectra measured with silicon drift detector EDS were quantified using the standards/matrix correction protocol embedded in the NIST DTSA-II software engine. Robust quantitative analytical results for trace constituents were obtained from concentrations as low as 0.000500 (mass fraction), even in the presence of significant peak interferences from minor (concentration 0.01≤C≤0.1) and major (C>0.1) constituents. Limits of detection as low as 0.000200 were achieved in the absence of peak interference.

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

NASA Astrophysics Data System (ADS)

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

2003-04-01

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

Electron microprobe analysis program for biological specimens: BIOMAP

NASA Technical Reports Server (NTRS)

Edwards, B. F.

1972-01-01

BIOMAP is a Univac 1108 compatible program which facilitates the electron probe microanalysis of biological specimens. Input data are X-ray intensity data from biological samples, the X-ray intensity and composition data from a standard sample and the electron probe operating parameters. Outputs are estimates of the weight percentages of the analyzed elements, the distribution of these estimates for sets of red blood cells and the probabilities for correlation between elemental concentrations. An optional feature statistically estimates the X-ray intensity and residual background of a principal standard relative to a series of standards.

Studies on the cellular and subcellular reactions in epidermis at irritant and allergic dermatitis.

PubMed

Lindberg, M

1982-01-01

To determine the cellular and subcellular reactions of keratinocytes at contact dermatitis, transmission electron microscopy was used in combination with energy dispersive X-ray microanalysis. Stereology and optical diffraction were used as complements to electron microscopy for studies of the effects of variations in the preparation technique on the ultrastructure of epidermis. The morphological effects of an increased hydration of epidermis were assessed by the use of occlusive patch tests. It was found that the relative volume of the epidermal intercellular space and the ultrastructure of the epidermal cells (keratinocytes and Langerhans' cells) were directly dependent on the osmolality of the fixative vehicle if glutaraldehyde was used as fixative. Cellular volume and morphology did also depend on the fixative used. Variations in the volume of the intercellular space were also detected when the water transport through epidermis was impaired by occlusive treatment. In normal epidermis prolonged fixation times (4 weeks) did not affect the morphology of the keratinocytes. However, if the structure and function of the keratinocytes were affected by the application of a irritant substance (DNCB), a loss of electron dense material from the cells was detected within 3 weeks. The ultrastructural changes in the keratinocytes at the irritant chromate and DNCB reactions were of a non-specific nature and are in accordance with the changes described for other irritant agents in the literature. A few cells with the features of apoptosis were recorded. The allergic chromate reaction was found to be a combination of the irritant reaction and a marked inflammatory response. To correlate the ultrastructural alterations in the keratinocytes with the functional state of the cells, X-ray microanalysis was used to determine the elemental redistribution occurring at the irritant DNCB reaction. The results of the X-ray microanalysis showed a good correlation between dose and time dependent effects and with the ultrastructural changes. Cell injury in the keratinocytes lead to decreases in the cellular content of phosphorous, potassium and magnesium and an increase of cellular calcium. Sodium, chloride, and sulphur were only moderately changed. A stimulation of the basal keratinocytes was detectable when a weak DNCB dose was applied to the skin.

Scanning electron microscopy/energy dispersive spectrometry fixedbeam or overscan x-ray microanalysis of particles can miss the real structure: x-ray spectrum image mapping reveals the true nature

NASA Astrophysics Data System (ADS)

Newbury, Dale E.; Ritchie, Nicholas W. M.

2013-05-01

The typical strategy for analysis of a microscopic particle by scanning electron microscopy/energy dispersive spectrometry x-ray microanalysis (SEM/EDS) is to use a fixed beam placed at the particle center or to continuously overscan to gather an "averaged" x-ray spectrum. While useful, such strategies inevitably concede any possibility of recognizing microstructure within the particle, and such fine scale structure is often critical for understanding the origins, behavior, and fate of particles. Elemental imaging by x-ray mapping has been a mainstay of SEM/EDS analytical practice for many years, but the time penalty associated with mapping with older EDS technology has discouraged its general use and reserved it more for detailed studies that justified the time investment. The emergence of the high throughput, high peak stability silicon drift detector (SDD-EDS) has enabled a more effective particle mapping strategy: "flash" x-ray spectrum image maps can now be recorded in seconds that capture the spatial distribution of major (concentration, C > 0.1 mass fraction) and minor (0.01 <= C <= 0.1) constituents. New SEM/SDD-EDS instrument configurations feature multiple SDDs that view the specimen from widely spaced azimuthal angles. Multiple, simultaneous measurements from different angles enable x-ray spectrometry and mapping that can minimize the strong geometric effects of particles. The NIST DTSA-II software engine is a powerful aid for quantitatively analyzing EDS spectra measured individually as well as for mapping information (available free for Java platforms at: http://www.cstl.nist.gov/div837/837.02/epq/dtsa2/index.html).

Chemical State Mapping of Degraded B4C Control Rod Investigated with Soft X-ray Emission Spectrometer in Electron Probe Micro-analysis.

PubMed

Kasada, R; Ha, Y; Higuchi, T; Sakamoto, K

2016-05-10

B4C is widely used as control rods in light water reactors, such as the Fukushima Daiichi nuclear power plant, because it shows excellent neutron absorption and has a high melting point. However, B4C can melt at lower temperatures owing to eutectic interactions with stainless steel and can even evaporate by reacting with high-temperature steam under severe accident conditions. To reduce the risk of recriticality, a precise understanding of the location and chemical state of B in the melt core is necessary. Here we show that a novel soft X-ray emission spectrometer in electron probe microanalysis can help to obtain a chemical state map of B in a modeled control rod after a high-temperature steam oxidation test.

Sample Preparation for Electron Probe Microanalysis—Pushing the Limits

PubMed Central

Geller, Joseph D.; Engle, Paul D.

2002-01-01

There are two fundamental considerations in preparing samples for electron probe microanalysis (EPMA). The first one may seem obvious, but we often find it is overlooked. That is, the sample analyzed should be representative of the population from which it comes. The second is a direct result of the assumptions in the calculations used to convert x-ray intensity ratios, between the sample and standard, to concentrations. Samples originate from a wide range of sources. During their journey to being excited under the electron beam for the production of x rays there are many possibilities for sample alteration. Handling can contaminate samples by adding extraneous matter. In preparation, the various abrasives used in sizing the sample by sawing, grinding and polishing can embed themselves. The most accurate composition of a contaminated sample is, at best, not representative of the original sample; it is misleading. Our laboratory performs EPMA analysis on customer submitted samples and prepares over 250 different calibration standards including pure elements, compounds, alloys, glasses and minerals. This large variety of samples does not lend itself to mass production techniques, including automatic polishing. Our manual preparation techniques are designed individually for each sample. The use of automated preparation equipment does not lend itself to this environment, and is not included in this manuscript. The final step in quantitative electron probe microanalysis is the conversion of x-ray intensities ratios, known as the “k-ratios,” to composition (in mass fraction or atomic percent) and/or film thickness. Of the many assumptions made in the ZAF (where these letters stand for atomic number, absorption and fluorescence) corrections the localized geometry between the sample and electron beam, or takeoff angle, must be accurately known. Small angular errors can lead to significant errors in the final results. The sample preparation technique then becomes very important, and, under certain conditions, may even be the limiting factor in the analytical uncertainty budget. This paper considers preparing samples to get known geometries. It will not address the analysis of samples with irregular, unprepared surfaces or unknown geometries. PMID:27446757

Enamel paint techniques in archaeology and their identification using XRF and micro-XRF

NASA Astrophysics Data System (ADS)

Hložek, M.; Trojek, T.; Komoróczy, B.; Prokeš, R.

2017-08-01

This investigation focuses in detail on the analysis of discoveries in South Moravia - important sites from the Roman period in Pasohlávky and Mušov. Using X-ray fluorescence analysis and micro-analysis we help identify the techniques of enamel paint and give a thorough chemical analysis in details which would not be possible to determine by means of macroscopic examination. We thus address the influence of elemental composition on the final colour of the enamel paint and describe the less known technique of combining enamel with millefiori. The material analyses of the metal artefacts decorated with enamel paint significantly contribute to our knowledge of the technology being used during the Roman period.

Development of synchrotron X-ray micro-tomography under extreme conditions of pressure and temperature.

PubMed

Álvarez-Murga, M; Perrillat, J P; Le Godec, Y; Bergame, F; Philippe, J; King, A; Guignot, N; Mezouar, M; Hodeau, J L

2017-01-01

X-ray tomography is a non-destructive three-dimensional imaging/microanalysis technique selective to a wide range of properties such as density, chemical composition, chemical states and crystallographic structure with extremely high sensitivity and spatial resolution. Here the development of in situ high-pressure high-temperature micro-tomography using a rotating module for the Paris-Edinburgh cell combined with synchrotron radiation is described. By rotating the sample chamber by 360°, the limited angular aperture of ordinary high-pressure cells is surmounted. Such a non-destructive high-resolution probe provides three-dimensional insight on the morphological and structural evolution of crystalline as well as amorphous phases during high pressure and temperature treatment. To demonstrate the potentials of this new experimental technique the compression behavior of a basalt glass is investigated by X-ray absorption tomography, and diffraction/scattering tomography imaging of the structural changes during the polymerization of C 60 molecules under pressure is performed. Small size and weight of the loading frame and rotating module means that this apparatus is portable, and can be readily installed on most synchrotron facilities to take advantage of the diversity of three-dimensional imaging techniques available at beamlines. This experimental breakthrough should open new ways for in situ imaging of materials under extreme pressure-temperature-stress conditions, impacting diverse areas in physics, chemistry, geology or materials sciences.

Internal iron biomineralization in Imperata cylindrica, a perennial grass: chemical composition, speciation and plant localization.

PubMed

Rodríguez, N; Menéndez, N; Tornero, J; Amils, R; de la Fuente, V

2005-03-01

* The analysis of metal distribution in Imperata cylindrica, a perennial grass isolated from the banks of Tinto River (Iberian Pyritic Belt), an extreme acidic environment with high content in metals, has shown a remarkable accumulation of iron. This property has been used to study iron speciation and its distribution among different tissues and structures of the plant. * Mossbauer (MS) and X-ray diffraction (XRD) were used to determine the iron species, scanning electron microscopy (SEM) to locate iron biominerals among plant tissue structures, and energy-dispersive X-ray microanalysis (EDAX), X-ray fluorescence (TXRF) and inductively coupled plasma emission spectroscopy (ICP-MS) to confirm their elemental composition. * The MS spectral analysis indicated that iron accumulated in this plant mainly as jarosite and ferritin. The presence of jarosite was confirmed by XRD and the distribution of both minerals in structures of different tissues was ascertained by SEM-EDAX analysis. * The convergent results obtained by complementary techniques suggest a complex iron management system in I. cylindrica, probably as a consequence of the environmental conditions of its habitat.

Kinetics and mechanism of the oxidation process of two-component Fe-Al alloys

NASA Technical Reports Server (NTRS)

Przewlocka, H.; Siedlecka, J.

1982-01-01

The oxidation process of two-component Fe-Al alloys containing up to 7.2% Al and from 18 to 30% Al was studied. Kinetic measurements were conducted using the isothermal gravimetric method in the range of 1073-1223 K and 1073-1373 K for 50 hours. The methods used in studies of the mechanism of oxidation included: X-ray microanalysis, X-ray structural analysis, metallographic analysis and marker tests.

Evaluating the Performance of a Commercial Silicon Drift Detector for X-ray Microanalysis

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

Kenik, Edward A

2011-01-01

Silicon drift detectors (SDDs) are rapidly becoming the energy dispersive spectrometer (EDS) of choice, especially for scanning electron microscopy x-ray microanalysis. The complementary features of large active areas (i.e., high collection angle) and high count rate capability of these detector contribute to their popularity, as well as the absence of liquid nitrogen cooling and good energy resolution of these detectors. The performance of an EDAX Apollo 40 SDD on a JEOL 6500F SEM is discussed. The larger detector resulted in an significant increase (~3.5x) in geometric collection efficiency compared to the original 10mm2 Si(Li) detector that it replaced. The SEMmore » can provide high beam currents (up to 200nA in some conditions) at small probe diameters. The high count rate capability of the SDD and the high current capability of the SEM compliment each other and provide excellent EDS analytical capabilities for both single point and spectrum imaging applications.« less

Influence of substrate material and surface finishing on the morphology of the calcium-phosphate coating.

PubMed

Leitão, E; Barbosa, M A; de Groot, K

1997-07-01

The formation of an apatite-like layer was achieved by immersing Ti-6A1-4V, Ti-Al-2.5Fe, and 316 L stainless-steel substrata in Hank's balanced salt solution (HBSS). The layer was characterized by surface analysis techniques, namely X-ray microanalysis and X-ray diffraction, and the morphology was observed by scanning electron microscopy and atomic force microscopy. The concentrations of Ca and P were monitored as a function of time. The morphology of the precipitate layer seems to be dependent both on the type of metal substrate and its surface finish. Polished Ti-6A1-4V and Ti-Al-2.5Fe surfaces exhibit a plate precipitate morphology, whereas rougher surfaces show scattered crystal-like precipitation. The results suggest that the layer produced by immersion of polished titanium alloys in HBSS is constituted by an amorphous apatite.

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

NASA Astrophysics Data System (ADS)

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

2017-10-01

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

Definition of the Spatial Resolution of X-Ray Microanalysis in Thin Foils

NASA Technical Reports Server (NTRS)

Williams, D. B.; Michael, J. R.; Goldstein, J. I.; Romig, A. D., Jr.

1992-01-01

The spatial resolution of X-ray microanalysis in thin foils is defined in terms of the incident electron beam diameter and the average beam broadening. The beam diameter is defined as the full width tenth maximum of a Gaussian intensity distribution. The spatial resolution is calculated by a convolution of the beam diameter and the average beam broadening. This definition of the spatial resolution can be related simply to experimental measurements of composition profiles across interphase interfaces. Monte Carlo calculations using a high-speed parallel supercomputer show good agreement with this definition of the spatial resolution and calculations based on this definition. The agreement is good over a range of specimen thicknesses and atomic number, but is poor when excessive beam tailing distorts the assumed Gaussian electron intensity distributions. Beam tailing occurs in low-Z materials because of fast secondary electrons and in high-Z materials because of plural scattering.

Electron probe microanalysis of calcium release and magnesium uptake by endoplasmic reticulum in bee photoreceptors

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

Baumann, O.; Walz, B.; Somlyo, A.V.

Honey bee photoreceptors contain large sacs of endoplasmic reticulum (ER) that can be located unequivocally in freeze-dried cryosections. The elemental compositon of the ER was determined by electron probe x-ray microanalysis and was visualized in high-resolution x-ray maps. In the ER of dark-adapted photoreceptors, the Ca concentration was 47.5 {plus minus} 1.1 mmol/kg (dry weight). During a 3-sec nonsaturating light stimulus, {approximately}50% of the Ca content was released from the ER. Light stimulation also caused a highly significant increase in the Mg content of the ER; the ratio of Mg uptake to Ca released was {approximately}0.7. Our results show unambiguouslymore » that the ER is the source of Ca{sup 2+} release during cell stimulation and suggest the Mg{sup 2+} can nearly balance the charge movement of Ca{sup 2+}.« less

Hydroxyapatite-armored poly(ε-caprolactone) microspheres and hydroxyapatite microcapsules fabricated via a Pickering emulsion route.

PubMed

Fujii, Syuji; Okada, Masahiro; Nishimura, Taiki; Maeda, Hayata; Sugimoto, Tatsuya; Hamasaki, Hiroyuki; Furuzono, Tsutomu; Nakamura, Yoshinobu

2012-05-15

Hydroxyapatite (HAp) nanoparticle-armored poly(ε-caprolactone) (PCL) microspheres were fabricated via a "Pickering-type" emulsion solvent evaporation method in the absence of any molecular surfactants. It was clarified that the interaction between carbonyl/carboxylic acid groups of PCL and the HAp nanoparticles at an oil-water interface played a crucial role in the preparation of the stable Pickering-type emulsions and the HAp nanoparticle-armored microspheres. The HAp nanoparticle-armored PCL microspheres were characterized in terms of size, size distribution, morphology, and chemical compositions using scanning electron microscopy, laser diffraction, energy dispersive X-ray microanalysis, and thermogravimetric analysis. The presence of HAp nanoparticles at the surface of the microspheres was confirmed by scanning electron microscopy and energy dispersive X-ray microanalysis. Pyrolysis of the PCL cores led to the formation of the corresponding HAp hollow microcapsules. Copyright © 2012 Elsevier Inc. All rights reserved.

Efforts to identify Te-rich nano-islands in ZnSe

NASA Astrophysics Data System (ADS)

Lau, June W.; Volkov, Vyacheslav V.; Zhu, Yimei; Kuskovsky, Igor L.; Neumark, Gertrude F.; Lin, W.; Maksimov, Oleg; Tamargo, Maria C.

2002-03-01

Much work has been done on the study of nano-island formation (“dopants”) in various systems by use of electron microscopy, often complemented by x-ray microanalysis [1]. This works well for systems involving one or more monolayers of dopants. Our system consists of Te and N dopants incorporated into ZnSe in sub-monolayer quantities [2]. This presents a challenge; our calculations show that this case is probably below the detection limit of x-ray microanalysis. Our samples do show strain contrasts but we were unable to obtain direct confirmation of nano-islands’ existence. As an alternative, dark field images from chemically sensitively reflections were used in volumetric defect density studies. The defect density in the doped samples was higher than that of the undoped samples. 1. Dorin C., U of Mich. Poster presentation at Fall MRS meeting 2001 2. Lin et al., Apple. Phys. Let., 76, 2205 (2000).

Electron probe X-ray microanalysis of cultured myogenic C2C12 cells with scanning and scanning transmission electron microscopy.

PubMed

Tylko, G; Karasiński, J; Wróblewski, R; Roomans, G M; Kilarski, W M

2000-01-01

Heterogeneity of the elemental content of myogenic C2C12 cultured cells was studied by electron probe X-ray microanalysis (EPXMA) with scanning (SEM EPXMA) and scanning transmission electron microscopy (STEM EPXMA). The best plastic substrate for growing cells was Thermanox. For STEM EPXMA, a Formvar film coated with carbon was found to be suitable substrate. The cells examined by scanning transmission electron microscopy showed great heterogeneity in their elemental content in comparison with the cells examined in the scanning electron microscope despite of an almost identical preparation procedure for EPXMA. Nevertheless the K/Na ratios obtained from both methods of EPXMA were very close (4.1 and 4.3). We conclude that the observed discrepancy in the elemental content obtained by the two methods may be due to differences in instrumentation and this must be taken into account when planning a comparative study.

Microstructure and properties of laser-clad high-temperature wear-resistant alloys

NASA Astrophysics Data System (ADS)

Yang, Yongqiang

1999-02-01

A 2-kW CO 2 laser with a powder feeder was used to produce alloy coatings with high temperature-wear resistance on the surface of steel substrates. To analyze the microstructure and microchemical composition of the laser-clad layers, a scanning electron microscope (SEM) equipped with an energy dispersive X-ray microanalysis system was employed. X-ray diffraction techniques were applied to characterize the phases formed during the cladding process. The results show that the microstructure of the cladding alloy consists mainly of many dispersed particles (W 2C, (W,Ti)C 1- x, WC), a lamellar eutectic carbide M 12C, and an (f.c.c) matrix. Hardness tested at room and high temperature showed that the laser-clad zone has a moderate room temperature hardness and relatively higher elevated temperature hardness. The application of the laser-clad layer to a hot tool was very successful, and its operational life span was prolonged 1 to 4 times.

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

Carreras, Alejo C., E-mail: acarreras@famaf.unc.edu.ar; Cangiano, María de los A.; Ojeda, Manuel W.

The influence of the amount of complexing agent added to the starting solution on the physicochemical properties of Cu–Ni nanostructured alloys obtained through a chemical route, was studied. For this purpose, three Cu–Ni nanoalloy samples were synthesized by a previously developed procedure, starting from solutions with citric acid to metal molar ratios (C/Me) of 0.73, 1.00 and 1.50. The synthesis technique consisted in preparing a precursor via the citrate-gel method, and carrying out subsequent thermal treatments in controlled atmospheres. Sample characterization was performed by scanning electron microscopy, X-ray microanalysis, X-ray diffraction, transmission electron microscopy, X-ray nanoanalysis and electron diffraction. Inmore » the three cases, copper and nickel formed a solid solution with a Cu/Ni atomic ratio close to 50/50, and free of impurities inside the crystal structure. The citric acid content of the starting solution proved to have an important influence on the morphology, size distribution, porosity, and crystallinity of the Cu–Ni alloy microparticles obtained, but a lesser influence on their chemical composition. The molar ratio C/Me = 1.00 resulted in the alloy with the Cu/Ni atomic ratio closest to 50/50. - Highlights: • We synthesize Cu–Ni nanoalloys by a chemical route based on the citrate-gel method. • We study the influence of the complexing agent content of the starting solution. • We characterize the samples by electron microscopy and X-ray techniques. • Citric acid influences the shape, size, porosity and crystallinity of the alloys.« less

Broadband high resolution X-ray spectral analyzer

DOEpatents

Silver, Eric H.; Legros, Mark; Madden, Norm W.; Goulding, Fred; Landis, Don

1998-01-01

A broad bandwidth high resolution x-ray fluorescence spectrometer has a performance that is superior in many ways to those currently available. It consists of an array of 4 large area microcalorimeters with 95% quantum efficiency at 6 keV and it produces x-ray spectra between 0.2 keV and 7 keV with an energy resolution of 7 to 10 eV. The resolution is obtained at input count rates per array element of 10 to 50 Hz in real-time, with analog pulse processing and thermal pile-up rejection. This performance cannot be matched by currently available x-ray spectrometers. The detectors are incorporated into a compact and portable cryogenic refrigerator system that is ready for use in many analytical spectroscopy applications as a tool for x-ray microanalysis or in research applications such as laboratory and astrophysical x-ray and particle spectroscopy.

Broadband high resolution X-ray spectral analyzer

DOEpatents

Silver, E.H.; Legros, M.; Madden, N.W.; Goulding, F.; Landis, D.

1998-07-07

A broad bandwidth high resolution X-ray fluorescence spectrometer has a performance that is superior in many ways to those currently available. It consists of an array of 4 large area microcalorimeters with 95% quantum efficiency at 6 keV and it produces X-ray spectra between 0.2 keV and 7 keV with an energy resolution of 7 to 10 eV. The resolution is obtained at input count rates per array element of 10 to 50 Hz in real-time, with analog pulse processing and thermal pile-up rejection. This performance cannot be matched by currently available X-ray spectrometers. The detectors are incorporated into a compact and portable cryogenic refrigerator system that is ready for use in many analytical spectroscopy applications as a tool for X-ray microanalysis or in research applications such as laboratory and astrophysical X-ray and particle spectroscopy. 6 figs.

Monte Carlo simulation of the effect of shape and thickness on SEM-EDS microanalysis of asbestos fibres and bundles: the case of anthophyllite, tremolite and actinolite

NASA Astrophysics Data System (ADS)

Valdrè, G.; Moro, D.; Ulian, G.

2018-01-01

Asbestos is a generic term used for six types of silicate minerals that are found in fibres or bundles of fibres, which can be easily cleaved into thinner ones. Scanning electron microscopy energy-dispersive X-ray spectrometry (SEM-EDS) quantitative microanalysis of asbestos mineral fibres still represents a complex analytical issue because of the variable fibre shape and small thickness (< 5 μm) compared with the penetration depth of the incident electron beam. Following previous work on chrysotile, crocidolite and amosite, here we present a study by means of Monte Carlo simulations of the thickness and shape effect on SEM-EDS microanalysis of anthophyllite, tremolite and actinolite asbestos. Realistic experimental conditions, such as sample geometry, SEM set-up and detector physics were taken into account. We report the results obtained on 100 μm long fibres and bundles of circular and square section and thicknesses from to 0.1 μm to 10 μm, for electron beam energies of 5, 15 and 25 keV. A strong influence of the asbestos mineral fibres and bundles shape and thickness on the detected EDS X-ray intensity was observed. In general, the X-ray intensities as a function of fibre thickness showed a considerable reduction below about 0.5 μm at 5 keV, 2 μm at 15 keV, and 5 μm at 25 keV for all the elements and minerals, with a non-linear dependence. Correction parameters, k-ratio, for the thickness effect were calculated and proposed.

Crystallization of the glassy phase of grain boundaries in silicon nitride

NASA Technical Reports Server (NTRS)

Jefferson, D. A.; Thomas, J. M.; Wen, S.

1984-01-01

Three types of hot-pressed silicon nitride specimens (containing 5wt% Y2O3 and 2wt% Al2O3 additives) which were subjected to different temperature heat treatments were studied by X-ray diffraction, X-ray microanalysis and high resolution electron microscopy. The results indicated that there were phase changes in the grain boundaries after heat treatment and the glassy phase at the grain boundaries was crystallized by heat treatment.

[In vitro study with techniques of imaging of the composition of urinary calculi].

PubMed

Tellez Martínez-Fornés, M; Burgos Revilla, F J; Sáez Garrido, J C; Soria Descalzo, J; Barbero González, J; Sánchez Corral, J; Minaya Minaya, A; Vallejo Herrador, J

1997-02-01

Pre-treatment knowledge of the lithiasic composition can be useful to design the most appropriate therapeutic scheme for each kind of stone. The relationship between the stone's densitometry information provided by the different imaging techniques, conventional radiology (RX), computerized axial tomography (CAT) and dual energy radiographic densitometry (DO) is analyzed, as well as the elemental composition determined by the microanalysis of fragments obtained post-lithotrity using a scanning electronic microscope (SEM) associated to X-ray dispersion energy (XDE). 60 stones, 12 for each pure composition selected (calcium oxalate mono and dihydro, phosphocarbonate, magnesium ammonium phosphate and uric acid), were studied with XR, CAT and DO and were later subjected to lithofragmentation in vitro. Fragments analysis was carried out post-lithotrity with SEM associated to XDE. The X-ray does not allow to establish the composition of some calculi. CAT quantifies the mineral contents of the oxalocalcic and infective calculi and differentiates the uric acid from the other compositions because the mean density values are under 500 Hounsfield Units. DO evaluates the lithiasic content in phosphocarbonate salts which are structurally similar to bone hydroxyapatite.

Procurement of novel microanalysis equipment for construction materials.

DOT National Transportation Integrated Search

2012-02-01

The equipment procured (i.e. an Orbis micro X-ray Fluorescence (MXRF) and an APSEX personal Scanning Electron Microscope (PSEM)) is part of the next generation of micro analytical equipment. These tools have the ability to make large volumes of...

Improvements in Electron-Probe Microanalysis: Applications to Terrestrial, Extraterrestrial, and Space-Grown Materials

NASA Technical Reports Server (NTRS)

Carpenter, Paul; Armstrong, John

2004-01-01

Improvement in the accuracy of electron-probe microanalysis (EPMA) has been accomplished by critical assessment of standards, correction algorithms, and mass absorption coefficient data sets. Experimental measurement of relative x-ray intensities at multiple accelerating potential highlights errors in the absorption coefficient. The factor method has been applied to the evaluation of systematic errors in the analysis of semiconductor and silicate minds. Accurate EPMA of Martian soil stimulant is necessary in studies that build on Martian rover data in anticipation of missions to Mars.

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

NASA Technical Reports Server (NTRS)

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

2002-01-01

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

From HeLa cell division to infectious diarrhoea

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

Stephen, J.; Osborne, M.P.; Spencer, A.J.

1990-09-01

Hela S3 cells were grown in suspension both randomly and, synchronously using hydroxyurea which blocks cells at the G1/S interface. Cryosections were prepared, freeze-dried and analyzed by X-ray microanalysis. As cells moved into S and through M phases (Na) and (Cl) increased; both returned to normal levels upon re-entering G1 phase. The Na/K ratio was 1:1 in G1 phase. Infection of HeLa S3 cells in G1 phase with vaccinia virus resulted in no change in intracellular (Na). Infection of neonatal mice with murine rotavirus was localized to villus tip enterocytes and gave rise to diarrhoea which was maximal at 72hmore » post-infection (p.i.). Diarrhoea was preceded by ischemia of villi (18-42h p.i.) and villus shortening (maximal at 42h p.i.), and was also coincident with a dramatic regrowth of villi. At 48h p.i. a proliferative zone of electron lucent cells was observed in villus base regions. Cryosections of infected gut, taken before, during, and after infection, together with corresponding age-matched controls, were freeze-dried and analysed by X-ray microanalysis. At 48h p.i. electron lucent villus base cells were shown to be more hydrated, and, to contain higher levels of both Na and Cl and lower levels of P, S, K and Mg than corresponding control cells. These studies increase confidence in the use of X-ray microanalysis in studying biological systems, provide some insight into the process of cell division, and constitute the basis of a new concept of diarrhoeal secretion.27 references.« less

Source Apportionment of Atmospheric Particles by Electron Probe X-Ray Microanalysis and Receptor Models.

NASA Astrophysics Data System (ADS)

van Borm, Werner August

Electron probe X-ray microanalysis (EPXMA) in combination with an automation system and an energy-dispersive X-ray detection system was used to analyse thousands of microscopical particles, originating from the ambient atmosphere. The huge amount of data was processed by a newly developed X-ray correction method and a number of data reduction procedures. A standardless ZAF procedure for EPXMA was developed for quick semi-quantitative analysis of particles starting from simple corrections, valid for bulk samples and modified taking into account the particle finit diameter, assuming a spherical shape. Tested on a limited database of bulk and particulate samples, the compromise between calculation speed and accuracy yielded for elements with Z > 14 accuracies on concentrations less than 10% while absolute deviations remained below 4 weight%, thus being only important for low concentrations. Next, the possibilities for the use of supervised and unsupervised multivariate particle classification were investigated for source apportionment of individual particles. In a detailed study of the unsupervised cluster analysis technique several aspects were considered, that have a severe influence on the final cluster analysis results, i.e. data acquisition, X-ray peak identification, data normalization, scaling, variable selection, similarity measure, cluster strategy, cluster significance and error propagation. A supervised approach was developed using an expert system-like approach in which identification rules are builded to describe the particle classes in a unique manner. Applications are presented for particles sampled (1) near a zinc smelter (Vieille-Montagne, Balen, Belgium), analyzed for heavy metals, (2) in an urban aerosol (Antwerp, Belgium), analyzed for over 20 elements and (3) in a rural aerosol originating from a swiss mountain area (Bern). Thus is was possible to pinpoint a number of known and unknown sources and characterize their emissions in terms of particles abundance and particle composition. Alternatively, the bulk analysis of filters (total, fine and coarse mode) using Particle Induced X -Ray Emission (PIXE) and the application of a receptor modeling approach provided for complementary information on a macroscopical level. A computer program was developed incorporating an absolute factor analysis based receptor modeling procedure. Source profiles and contributions are described by elemental concentrations and an atmospheric mass balance is put forward. The latter method was applied in a two year study of the Antwerp urban aerosol and for the swiss aerosol, revealing a number of previously known and unknown sources. Both methods were successfully combined to increase the source resolution.

Chromium distribution in shoots of macrophyte Callitriche cophocarpa Sendtn.

PubMed

Augustynowicz, Joanna; Wróbel, Paweł; Płachno, Bartosz J; Tylko, Grzegorz; Gajewski, Zbigniew; Węgrzynek, Dariusz

2014-06-01

The aim of the study was the analysis of Cr distribution in shoots of the macrophyte Callitriche cophocarpa by means of two X-ray-based techniques: micro X-ray fluorescence (μXRF) and electron probe X-ray microanalysis (EPXMA). Plants were treated with 100 μM (5.2 mg l(-1)) chromium solutions for 7 days. Cr was introduced independently at two speciations as Cr(III) and Cr(VI), known for their diverse physicochemical properties and different influence on living organisms. A comparative analysis of Cr(III)-treated plants by EPXMA and μXRF demonstrated high deposition of Cr in epidermal glands/hairs localized on leaves and stems of the plant shoots. Cr in Cr(III)-treated plants was recorded solely in glands/hairs, and the element was not present in any other structures. On the other hand, Cr in Cr(VI)-treated group of plants was rather found in vascular bundles. Moreover, the concentration of Cr in Cr(VI)-treated plants was significantly lower than in plants incubated in Cr(III) solution. The results obtained in this work suggest differences in chromium uptake, transport and accumulation dependent on the oxidative state of the element.

μ-SRXRF characterization of Brazilian emeralds

NASA Astrophysics Data System (ADS)

Curado, J. F.; Radtke, M.; Buzanich, G.; Reinholz, U.; Riesemeier, H.; Guttler, R. A. S.; Rizzutto, M. A.

2014-04-01

The aim of the present study is to characterize emeralds from different mines of Brazil by using Synchrotron Radiation X-ray Fluorescence Microanalysis (μ-SRXRF). The advantage of this technique is that we can analyze a homogeneous, inclusion free area of the stone with the microbeam to distinguish the elemental fingerprint according to the provenance of the emerald. A total of 47 samples belonging to 5 different Brazilian mines were studied in this work and 28 elements were identified. By means of Principal Component Analysis (PCA) it is possible to build different groups according to the provenance of the stones, which allows to assign samples of unknown origin to the according mine.

Bone fragments a body can make

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

Stout, S.D.; Ross, L.M. Jr.

Data obtained from various analytical techniques applied to a number of small bone fragments recovered from a crime scene were used to provide evidence for the occurrence of a fatality. Microscopic and histomorphometric analyses confirmed that the fragments were from a human skull. X-ray microanalysis of darkened areas on the bone fragments revealed a chemical signature that matched the chemical signature of a shotgun pellet recovered at the scene of the crime. The above findings supported the deoxyribonucleic acid (DNA) fingerprint evidence which, along with other evidence, was used to convict a man for the murder of his wife, evenmore » though her body was never recovered.« less

Comparative Analysis of Microbial Communities in Iron-Dominated Flocculent Mats in Deep-Sea Hydrothermal Environments

PubMed Central

Kikuchi, Sakiko; Mitsunobu, Satoshi; Takaki, Yoshihiro; Yamanaka, Toshiro; Toki, Tomohiro; Noguchi, Takuroh; Nakamura, Kentaro; Abe, Mariko; Hirai, Miho; Yamamoto, Masahiro; Uematsu, Katsuyuki; Miyazaki, Junichi; Nunoura, Takuro; Takahashi, Yoshio; Takai, Ken

2016-01-01

ABSTRACT It has been suggested that iron is one of the most important energy sources for photosynthesis-independent microbial ecosystems in the ocean crust. Iron-metabolizing chemolithoautotrophs play a key role as primary producers, but little is known about their distribution and diversity and their ecological role as submarine iron-metabolizing chemolithotrophs, particularly the iron oxidizers. In this study, we investigated the microbial communities in several iron-dominated flocculent mats found in deep-sea hydrothermal fields in the Mariana Volcanic Arc and Trough and the Okinawa Trough by culture-independent molecular techniques and X-ray mineralogical analyses. The abundance and composition of the 16S rRNA gene phylotypes demonstrated the ubiquity of zetaproteobacterial phylotypes in iron-dominated mat communities affected by hydrothermal fluid input. Electron microscopy with energy-dispersive X-ray microanalysis and X-ray absorption fine structure (XAFS) analysis revealed the chemical and mineralogical signatures of biogenic Fe-(oxy)hydroxide species and the potential contribution of Zetaproteobacteria to the in situ generation. These results suggest that putative iron-oxidizing chemolithoautotrophs play a significant ecological role in producing iron-dominated flocculent mats and that they are important for iron and carbon cycles in deep-sea low-temperature hydrothermal environments. IMPORTANCE We report novel aspects of microbiology from iron-dominated flocculent mats in various deep-sea environments. In this study, we examined the relationship between Zetaproteobacteria and iron oxides across several hydrothermally influenced sites in the deep sea. We analyzed iron-dominated mats using culture-independent molecular techniques and X-ray mineralogical analyses. The scanning electron microscopy–energy-dispersive X-ray spectroscopy SEM-EDS analysis and X-ray absorption fine structure (XAFS) analysis revealed chemical and mineralogical signatures of biogenic Fe-(oxy)hydroxide species as well as the potential contribution of the zetaproteobacterial population to the in situ production. These key findings provide important information for understanding the mechanisms of both geomicrobiological iron cycling and the formation of iron-dominated mats in deep-sea hydrothermal fields. PMID:27422841

Chemometric classification of gunshot residues based on energy dispersive X-ray microanalysis and inductively coupled plasma analysis with mass-spectrometric detection

NASA Astrophysics Data System (ADS)

Steffen, S.; Otto, M.; Niewoehner, L.; Barth, M.; Bro¿żek-Mucha, Z.; Biegstraaten, J.; Horváth, R.

2007-09-01

A gunshot residue sample that was collected from an object or a suspected person is automatically searched for gunshot residue relevant particles. Particle data (such as size, morphology, position on the sample for manual relocation, etc.) as well as the corresponding X-ray spectra and images are stored. According to these data, particles are classified by the analysis-software into different groups: 'gunshot residue characteristic', 'consistent with gunshot residue' and environmental particles, respectively. Potential gunshot residue particles are manually checked and - if necessary - confirmed by the operating forensic scientist. As there are continuing developments on the ammunition market worldwide, it becomes more and more difficult to assign a detected particle to a particular ammunition brand. As well, the differentiation towards environmental particles similar to gunshot residue is getting more complex. To keep external conditions unchanged, gunshot residue particles were collected using a specially designed shooting device for the test shots revealing defined shooting distances between the weapon's muzzle and the target. The data obtained as X-ray spectra of a number of particles (3000 per ammunition brand) were reduced by Fast Fourier Transformation and subjected to a chemometric evaluation by means of regularized discriminant analysis. In addition to the scanning electron microscopy in combination with energy dispersive X-ray microanalysis results, isotope ratio measurements based on inductively coupled plasma analysis with mass-spectrometric detection were carried out to provide a supplementary feature for an even lower risk of misclassification.

Direct observation of nitrate and sulfate formations from mineral dust and sea-salts using low- Z particle electron probe X-ray microanalysis

NASA Astrophysics Data System (ADS)

Hwang, HeeJin; Ro, Chul-Un

In the present work, it is demonstrated that a single particle analytical technique, named low- Z particle electron probe X-ray microanalysis, is a practically useful tool for the study of heterogeneous reactions of mineral dust and sea-salts when this analytical technique was applied to a sample collected during an Asian Dust storm event. The technique does not require a special treatment of sample to identify particles reacted in the air. Also, quantitative chemical speciation of reacted particles can provide concrete information on what chemical reaction, if any, occurred for individual particles. Among overall 178 analyzed particles, the number of reacted particles is 81 and heterogeneous chemical reactions mostly occurred on CaCO 3 mineral dust (54 particles) and sea-salts (26 particles). Several observations made for the Asian Dust sample in the present work are: (1) CaCO 3 species almost completely reacted to produce mostly Ca(NO 3) 2 species, and CaSO 4 to a much lesser extent. (2) When reacted particles contain CaSO 4, almost all of them are internally mixed with nitrate. (3) Reacted CaCO 3 particles seem to contain moisture when they were collected. (4) Some reacted CaCO 3 particles have unreacted mineral species, such as aluminosilicates, iron oxide, SiO 2, etc., in the core region. (5) All sea-salt particles are observed to have reacted in the air. Some of them were recrystallized in the air before being collected and they are observed as crystalline NaNO 3 particles. (6) Many sea-salts were collected as water drops, and some of them were fractionally recrystallized on Ag collecting substrate. When sea-salts were not recrystallized on the substrate, they are found as particles internally mixed with NaNO 3 and Mg(NO 3) 2, and in some cases SO 4 and Cl species as additional anions.

Scanning Electron Microanalysis and Analytical Challenges of Mapping Elements in Urban Atmospheric Particles

EPA Science Inventory

Elemental mapping with energy-dispersive X-ray spectroscopy (EDX) associated with scanning electron microscopy is highly useful for studying internally mixed atmospheric particles. Presented is a study of individual particles from urban airsheds and the analytical challenges in q...

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

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

Jin, Qiaoling; Vogt, Stefan; Lai, Barry

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

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

DOE PAGES

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

2015-02-23

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

Subcellular distribution of an inhalational anesthetic in situ

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

Eckenhoff, R.G.; Shuman, H.

1990-01-01

To better understand the mechanisms and sites of anesthetic action, we determined the subcellular partitioning of halothane in a tissue model. A method was found to fix the in vivo distribution of halothane in rat atrial tissue for subsequent electron microscopy and x-ray microanalysis. Atrial strips were exposed to various concentrations of halothane, rapidly frozen, cryo-sectioned, and cryo-transferred into an electron microscope. Irradiation of the hydrated cryosections with the electron beam caused halothane radiolysis, which allowed retention of the halogen-containing fragments after dehydration of the sections. The bromine from halothane was detected and quantified with x-ray microanalysis in various microregionsmore » of atrial myocytes. Halothane (bromine) partitioned largely to mitochondria, with progressively lower concentrations in sarcolemma, nuclear membrane, cytoplasm, sarcomere, and nucleus. Partitioning could not be explained solely by distribution of cellular lipid, suggesting significant and differential physicochemical solubility in protein. However, we found no saturable compartment in atrial myocytes within the clinical concentration range, which implies little specific protein binding.« less

Effect of Gold on the Microstructural Evolution and Integrity of a Sintered Silver Joint

NASA Astrophysics Data System (ADS)

Muralidharan, Govindarajan; Leonard, Donovan N.; Meyer, Harry M.

2017-07-01

There is a need for next-generation, high-performance power electronic packages and systems employing wide-bandgap devices to operate at high temperatures in automotive and electric grid applications. Sintered silver joints are currently being evaluated as an alternative to Pb-free solder joints. Of particular interest is the development of joints based on silver paste consisting of nano- or micron-scale particles that can be processed without application of external pressure. The microstructural evolution at the interface of a pressureless-sintered silver joint formed between a SiC die with Ti/Ni/Au metallization and an active metal brazed (AMB) substrate with Ag metallization at 250°C has been evaluated using scanning electron microscopy (SEM), x-ray microanalysis, and x-ray photoelectron spectroscopy (XPS). Results from focused ion beam (FIB) cross-sections show that, during sintering, pores in the sintered region near to the Au layer tend to be narrow and elongated with long axis oriented parallel to the interface. Further densification results in formation of many small, relatively equiaxed pores aligned parallel to the interface, creating a path for easy crack propagation. X-ray microanalysis results confirm interdiffusion between Au and Ag and that a region with poor mechanical strength is formed at the edge of this region of interdiffusion.

Interfacial microanalysis of rubber tyre-cord adhesion and the influence of cobalt

NASA Astrophysics Data System (ADS)

Fulton, W. Stephen; Smith, Graham C.; Titchener, Keith J.

2004-01-01

The effect of cobalt-containing adhesion promoters on the structure and morphology of rubber-brass and rubber-tyre-cord interfaces before and after ageing has been investigated by X-ray photoelectron spectroscopy (XPS) depth profiling, glancing incidence X-ray diffraction (XRD) and transmission electron microscopy (TEM). The effect the cobalt adhesion promoters had upon the interface morphology as they suppressed the growth of crystalline dendrites normally associated with the ageing process was imaged in TEM using samples prepared by the focused ion beam (FIB) milling technique. XPS depth profiling through the interfaces revealed that different types of adhesion promoter influenced the amount and distribution of cobalt ions in the bonding layer. XRD demonstrated the influence that cobalt had upon the structure of the interface and subsequent crystallinity, with a lesser degree of crystallinity being associated with better adhesion performance. From the results a model for the effect of the Co chemistry of the adhesion promotor has been developed.

Spectroscopic, microchemical and petrographic analyses of plasters from ancient buildings in Lamezia Terme (Calabria, Southern Italy)

NASA Astrophysics Data System (ADS)

De Luca, Raffaella; Gigliotti, Valentina; Panarello, Mario; Bloise, Andrea; Crisci, Gino M.; Miriello, Domenico

2016-01-01

This work shows the results of the spectroscopic, microchemical and petrographic study carried out on six plasters coming from three important residential buildings of the 18th century, located in Lamezia Terme (Catanzaro, Southern Italy). To study the provenance of the raw materials used to make the plasters, one sample of limestone and two samples of sand were also collected from the quarries near Lamezia Terme and compared with the historical plasters. Samples were studied by polarized optical microscopy (OM), X-ray powder diffraction (XRPD), scanning electron microscopy (SEM) with energy dispersive X-ray spectroscopy (EDS) and Raman spectroscopy. The results of these analyses allowed to determine the mineralogical, petrographical and chemical characteristics of the plasters, identify the pigments used for their coloration and provide useful information about the building techniques, the raw materials employed and the production technology of plasters during the 18th century in Lamezia Terme. SEM-EDS microanalysis also revealed the presence of gold and silver on the surface of two samples.

Green Synthesis and Characterization of SmVO4 Nanoparticles in the Presence of Carbohydrates As Capping Agents with Investigation of Visible-Light Photocatalytic Properties

NASA Astrophysics Data System (ADS)

Eghbali-Arani, Mohammad; Sobhani-Nasab, Ali; Rahimi-Nasrabadi, Mehdi; Pourmasoud, Saeid

2018-03-01

SmVO4 nanoparticles were synthesized through a fast and simple procedure (green method). The effects of three parameters including temperature, type of capping agent, and concentration on the size and morphology behavior of SmVO4 nanoparticles were explored. The analysis of SmVO4 nanoparticles was performed through some techniques including, Fourier transform infrared spectroscopy, x-ray diffraction, energy dispersive x-ray microanalysis, scanning electron microscopy, transmission electron microscopy, thermogravimetry, differential thermal analysis, ultraviolet-visible spectroscopy, and vibrating sample magnetometers. The study of photocatalytic behaviour of the SmVO4 nanoparticles in various conditions has been carried out. The impacts of different factors such as dosage, grain size, and kind of pollutant (methylene blue = MB and methyl orange = MO) on the photocatalytic property of SmVO4 nanoparticles were assessed. The photocatalytic activities of SmVO4 catalysts were studied for the degradation of dye under visible light (λ > 400 nm).

Preparation of nanostructured and nanosheets of MoS2 oxide using oxidation method.

PubMed

Amini, Majed; Ramazani S A, Ahmad; Faghihi, Morteza; Fattahpour, Seyyedfaridoddin

2017-11-01

Molybdenum disulfide (MoS 2 ), a two-dimensional transition metal has a 2D layered structure and has recently attracted attention due to its novel catalytic properties. In this study, MoS 2 has been successfully intercalated using chemical and physical intercalation techniques, while enhancing its surface properties. The final intercalated MoS 2 is of many interests because of its low-dimensional and potential properties in in-situ catalysis. In this research, we report different methods to intercalate the layers of MoS 2 successfully using acid-treatment, ultrasonication, oxidation and thermal shocking. The other goal of this study is to form SO bonds mainly because of expected enhanced in-situ catalytic operations. The intercalated MoS 2 is further characterized using analyses such as Fourier Transform Infrared Spectroscopy (FTIR), Raman, Contact Angle, X-ray diffraction (XRD), Field Emission Scanning Electron Microscope (FESEM), Energy Dispersive X-Ray Microanalysis (EDAX), Transmission electron microscopy (TEM), and BET. Copyright © 2017. Published by Elsevier B.V.

ITEP MEVVA ion beam for rhenium silicide production.

PubMed

Kulevoy, T; Gerasimenko, N; Seleznev, D; Kropachev, G; Kozlov, A; Kuibeda, R; Yakushin, P; Petrenko, S; Medetov, N; Zaporozhan, O

2010-02-01

The rhenium silicides are very attractive materials for semiconductor industry. In the Institute for Theoretical and Experimental Physics (ITEP) at the ion source test bench the research program of rhenium silicide production by ion beam implantation are going on. The investigation of silicon wafer after implantation of rhenium ion beam with different energy and with different total dose were carried out by secondary ions mass spectrometry, energy-dispersive x-ray microanalysis, and x-ray diffraction analysis. The first promising results of rhenium silicide film production by high intensity ion beam implantation are presented.

Characterization and speciation of mercury-bearing mine wastes using X-ray absorption spectroscopy

USGS Publications Warehouse

Kim, C.S.; Brown, Gordon E.; Rytuba, J.J.

2000-01-01

Mining of mercury deposits located in the California Coast Range has resulted in the release of mercury to the local environment and water supplies. The solubility, transport, and potential bioavailability of mercury are controlled by its chemical speciation, which can be directly determined for samples with total mercury concentrations greater than 100 mg kg-1 (ppm) using X-ray absorption spectroscopy (XAS). This technique has the additional benefits of being non-destructive to the sample, element-specific, relatively sensitive at low concentrations, and requiring minimal sample preparation. In this study, Hg L(III)-edge extended X-ray absorption fine structure (EXAFS) spectra were collected for several mercury mine tailings (calcines) in the California Coast Range. Total mercury concentrations of samples analyzed ranged from 230 to 1060 ppm. Speciation data (mercury phases present and relative abundances) were obtained by comparing the spectra from heterogeneous, roasted (calcined) mine tailings samples with a spectral database of mercury minerals and sorbed mercury complexes. Speciation analyses were also conducted on known mixtures of pure mercury minerals in order to assess the quantitative accuracy of the technique. While some calcine samples were found to consist exclusively of mercuric sulfide, others contain additional, more soluble mercury phases, indicating a greater potential for the release of mercury into solution. Also, a correlation was observed between samples from hot-spring mercury deposits, in which chloride levels are elevated, and the presence of mercury-chloride species as detected by the speciation analysis. The speciation results demonstrate the ability of XAS to identify multiple mercury phases in a heterogeneous sample, with a quantitative accuracy of ??25% for the mercury-containing phases considered. Use of this technique, in conjunction with standard microanalytical techniques such as X-ray diffraction and electron probe microanalysis, is beneficial in the prioritization and remediation of mercury-contaminated mine sites. (C) 2000 Elsevier Science B.V.

Use of scanning electron microscopy and microanalysis to determine chloride content of concrete and raw materials.

DOT National Transportation Integrated Search

2013-02-01

Standard sample sets of cement and mortar formulations with known levels of Cl as well as concrete samples subject to Cl diffusion were all prepared for and analyzed with scanning electron microscopy (SEM) and electron microprobe (EPMA). Using x-ray ...

Determination of low-Z elements in individual environmental particles using windowless EPMA.

PubMed

Ro, C U; Osán, J; Van Grieken, R

1999-04-15

The determination of low-Z elements such as carbon, nitrogen, and oxygen in atmospheric aerosol particles is of interest in studying environmental pollution. Conventional electron probe microanalysis technique has a limitation for the determination of the low-Z elements, mainly because the Be window in an energy-dispersive X-ray (EDX) detector hinders the detection of characteristic X-rays from light elements. The feasibility of low-Z element determination in individual particles using a windowless EDX detector is investigated. To develop a method capable of identifying chemical species of individual particles, both the matrix and the geometric effects of particles have to be evaluated. X-rays of low-Z elements generated by an electron beam are so soft that important matrix effects, mostly due to X-ray absorption, exist even within particles in the micrometer size range. Also, the observed radiation, especially that of light elements, experiences different extents of absorption, depending on the shape and size of the particles. Monte Carlo calculation is applied to explain the variation of observed X-ray intensities according to the geometric and chemical compositional variation of individual particles, at different primary electron beam energies. A comparison is carried out between simulated and experimental data, collected for standard individual particles with chemical compositions as generally observed in marine and continental aerosols. Despite the many fundamental problematic analytical factors involved in the observation of X-rays from low-Z elements, the Monte Carlo calculation proves to be quite reliable to evaluate those matrix and geometric effects. Practical aspects of the Monte Carlo calculation for the determination of light elements in individual particles are also considered.

Using DTSA-II to simulate and interpret energy dispersive spectra from particles.

PubMed

Ritchie, Nicholas W M

2010-06-01

A high quality X-ray spectrum image of a 3.3 mum diameter sphere of K411 glass resting on a copper substrate was collected at 25 keV. The same sample configuration was modeled using the NISTMonte Monte Carlo simulation of electron and X-ray transport as is integrated into the quantitative X-ray microanalysis software package DTSA-II. The distribution of measured and simulated X-ray intensity compare favorably for all the major lines present in the spectra. The simulation is further examined to investigate the influence of angle-of-incidence, sample thickness, and sample diameter on the generated and measured X-ray intensity. The distribution of generated X-rays is seen to deviate significantly from a naive model which assumes that the distribution of generated X-rays is similar to bulk within the volume they share in common. It is demonstrated that the angle at which the electron beam strikes the sample has nonnegligible consequences. It is also demonstrated that within the volume that the bulk and particle share in common that electrons, which have exited and later reentered the particle volume, generate a significant fraction of the X-rays. Any general model of X-ray generation in particles must take into account the lateral spread of the scattered electron beam.

The reserpinized rat in the study of cystic fibrosis: x-ray microanalysis of submandibular gland and pancreas

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

Roomans, G.M.; Wei, X.; Ceder, O.

The chronically reserpinized rat has been suggested as an animal model for cystic fibrosis. X-ray microanalysis of thick and thin cryosections was carried out to assess elemental redistribution in the submandibular glands and the pancreas of reserpinized rats at the cellular and subcellular level. In the submandibular gland of reserpinized rats, calcium and magnesium concentrations were significantly elevated. Mucus globules, secretory granules, and endoplasmic reticulum were the primary sites of the localization of excess calcium and magnesium. A significant potassium loss from the gland had occurred, particularly from the serous cells. Electron microscopy of conventionally prepared tissue showed marked swellingmore » of the endoplasmic reticulum, especially in mucous cells. The elemental changes in the pancreatic acinar cells of reserpinized rats were reminiscent of elemental redistribution connected with cell death: increased levels of sodium, chlorine, and calcium and decreased levels of magnesium and potassium. Ultrastructural changes included swelling of the endoplasmic reticulum and obstruction of the acinar lumen. It is concluded tha elemental redistribution in chronically reserpinized rats presents interesting parallels with cystic fibrosis.« less

FIB preparation of a NiO Wedge-Lamella and STEM X-ray microanalysis for the determination of the experimental k(O-Ni) Cliff-Lorimer coefficient.

PubMed

Armigliato, Aldo; Frabboni, Stefano; Gazzadi, Gian Carlo; Rosa, Rodolfo

2013-02-01

A method for the fabrication of a wedge-shaped thin NiO lamella by focused ion beam is reported. The starting sample is an oxidized bulk single crystalline, <100> oriented, Ni commercial standard. The lamella is employed for the determination, by analytical electron microscopy at 200 kV of the experimental k(O-Ni) Cliff-Lorimer (G. Cliff & G.W. Lorimer, J Microsc 103, 203-207, 1975) coefficient, according to the extrapolation method by Van Cappellen (E. Van Cappellen, Microsc Microstruct Microanal 1, 1-22, 1990). The result thus obtained is compared to the theoretical k(O-Ni) values either implemented into the commercial software for X-ray microanalysis quantification of the scanning transmission electron microscopy/energy dispersive spectrometry equipment or calculated by the Monte Carlo method. Significant differences among the three values are found. This confirms that for a reliable quantification of binary alloys containing light elements, the choice of the Cliff-Lorimer coefficients is crucial and experimental values are recommended.

The detection of sulphur in contamination spots in electron probe X-ray microanalysis

USGS Publications Warehouse

Adler, I.; Dwornik, E.J.; Rose, H.J.

1962-01-01

Sulphur has been identified as one of the elements present in the contamination spot which forms under the electron beam in the microprobe. The presence of the sulphur results in a rapid change in intensity measurements causing a loss of observed intensity for elements other than sulphur. The source of sulphur has been traced at least in part to the Apiezon B diffusion pump oil. A comparative X-ray fluorescence study of the Apiezon B and Octoil diffusion pump oils showed substantial amounts of sulphur in the Apiezon B. The Octoil was relatively free of sulphur.

Chromium mapping in male mice reproductive glands exposed to CrCl 3 using proton and X-ray synchrotron radiation microbeams

NASA Astrophysics Data System (ADS)

Ortega, R.; Devès, G.; Bonnin-Mosbah, M.; Salomé, M.; Susini, J.; Anderson, L. M.; Kasprzak, K. S.

2001-07-01

Preconception exposure to certain chemicals may increase risk of tumors in offspring, especially with regard to occupational metals such as chromium. However, the mechanism of chromium trans-generation carcinogenicity remains unknown. Using scanning proton X-ray microanalysis we have been able to detect chromium in testicular tissue sections from mice treated by intraperitoneal injection of 1 mmol/kg CrCl 3. Chromium concentration was about 5 μg/g dry mass in average, but higher concentrations were found within the limiting membrane of the testes, the tunica albuginea. In addition, synchrotron radiation X-ray fluorescence measurements, with microscopic resolution, clearly demonstrated the presence of chromium in the tunica albuginea but also within isolated cells from the interstitial connective tissue.

Comparative Analysis of Microbial Communities in Iron-Dominated Flocculent Mats in Deep-Sea Hydrothermal Environments.

PubMed

Makita, Hiroko; Kikuchi, Sakiko; Mitsunobu, Satoshi; Takaki, Yoshihiro; Yamanaka, Toshiro; Toki, Tomohiro; Noguchi, Takuroh; Nakamura, Kentaro; Abe, Mariko; Hirai, Miho; Yamamoto, Masahiro; Uematsu, Katsuyuki; Miyazaki, Junichi; Nunoura, Takuro; Takahashi, Yoshio; Takai, Ken

2016-10-01

It has been suggested that iron is one of the most important energy sources for photosynthesis-independent microbial ecosystems in the ocean crust. Iron-metabolizing chemolithoautotrophs play a key role as primary producers, but little is known about their distribution and diversity and their ecological role as submarine iron-metabolizing chemolithotrophs, particularly the iron oxidizers. In this study, we investigated the microbial communities in several iron-dominated flocculent mats found in deep-sea hydrothermal fields in the Mariana Volcanic Arc and Trough and the Okinawa Trough by culture-independent molecular techniques and X-ray mineralogical analyses. The abundance and composition of the 16S rRNA gene phylotypes demonstrated the ubiquity of zetaproteobacterial phylotypes in iron-dominated mat communities affected by hydrothermal fluid input. Electron microscopy with energy-dispersive X-ray microanalysis and X-ray absorption fine structure (XAFS) analysis revealed the chemical and mineralogical signatures of biogenic Fe-(oxy)hydroxide species and the potential contribution of Zetaproteobacteria to the in situ generation. These results suggest that putative iron-oxidizing chemolithoautotrophs play a significant ecological role in producing iron-dominated flocculent mats and that they are important for iron and carbon cycles in deep-sea low-temperature hydrothermal environments. We report novel aspects of microbiology from iron-dominated flocculent mats in various deep-sea environments. In this study, we examined the relationship between Zetaproteobacteria and iron oxides across several hydrothermally influenced sites in the deep sea. We analyzed iron-dominated mats using culture-independent molecular techniques and X-ray mineralogical analyses. The scanning electron microscopy-energy-dispersive X-ray spectroscopy SEM-EDS analysis and X-ray absorption fine structure (XAFS) analysis revealed chemical and mineralogical signatures of biogenic Fe-(oxy)hydroxide species as well as the potential contribution of the zetaproteobacterial population to the in situ production. These key findings provide important information for understanding the mechanisms of both geomicrobiological iron cycling and the formation of iron-dominated mats in deep-sea hydrothermal fields. Copyright © 2016, American Society for Microbiology. All Rights Reserved.

A flexible and accurate quantification algorithm for electron probe X-ray microanalysis based on thin-film element yields

NASA Astrophysics Data System (ADS)

Schalm, O.; Janssens, K.

2003-04-01

Quantitative analysis by means of electron probe X-ray microanalysis (EPXMA) of low Z materials such as silicate glasses can be hampered by the fact that ice or other contaminants build up on the Si(Li) detector beryllium window or (in the case of a windowless detector) on the Si(Li) crystal itself. These layers act as an additional absorber in front of the detector crystal, decreasing the detection efficiency at low energies (<5 keV). Since the layer thickness gradually changes with time, also the detector efficiency in the low energy region is not constant. Using the normal ZAF approach to quantification of EPXMA data is cumbersome in these conditions, because spectra from reference materials and from unknown samples must be acquired within a fairly short period of time in order to avoid the effect of the change in efficiency. To avoid this problem, an alternative approach to quantification of EPXMA data is proposed, following a philosophy often employed in quantitative analysis of X-ray fluorescence (XRF) and proton-induced X-ray emission (PIXE) data. This approach is based on the (experimental) determination of thin-film element yields, rather than starting from infinitely thick and single element calibration standards. These thin-film sensitivity coefficients can also be interpolated to allow quantification of elements for which no suitable standards are available. The change in detector efficiency can be monitored by collecting an X-ray spectrum of one multi-element glass standard. This information is used to adapt the previously determined thin-film sensitivity coefficients to the actual detector efficiency conditions valid on the day that the experiments were carried out. The main advantage of this method is that spectra collected from the standards and from the unknown samples should not be acquired within a short period of time. This new approach is evaluated for glass and metal matrices and is compared with a standard ZAF method.

Chemically prepared La2Se3 nanocubes thin film for supercapacitor application.

PubMed

Patil, S J; Lokhande, V C; Chodankar, N R; Lokhande, C D

2016-05-01

Lanthanum selenide (La2Se3) nanocubes thin film is prepared via successive ionic layer adsorption and reaction (SILAR) method and utilized for energy storage application. The prepared La2Se3 thin film is characterized by X-ray diffraction, field emission scanning electron microscopy and contact angle measurement techniques for structural, surface morphological and wettability studies, respectively. Energy dispersive X-ray microanalysis (EDAX) is performed in order to obtain the elemental composition of the thin film. The La2Se3 film electrode shows a maximum specific capacitance of 363 F g(-1) in a 0.8 M LiClO4/PC electrolyte at a scan rate of 5 mV s(-1) within 1.3 V/SCE potential range. The specific capacitive retention of 83 % of La2Se3 film electrode is obtained over 1000 cyclic voltammetry cycles. The predominant performance, such as high energy (80 Wh kg(-1)) and power density (2.5 kW kg(-1)), indicates that La2Se3 film electrode facilitates fast ion diffusion during redox processes. Copyright © 2016 Elsevier Inc. All rights reserved.

Scanning Electron Microscopy and X-Ray Microanalysis for Chemical and Morphological Characterisation of the Inorganic Component of Gunshot Residue: Selected Problems

PubMed Central

Brożek-Mucha, Zuzanna

2014-01-01

Chosen aspects of examinations of inorganic gunshot particles by means of scanning electron microscopy and energy dispersive X-ray spectrometry technique are presented. The research methodology of particles was worked out, which included a precise and repeatable procedure of the automatic detection and identification of particles as well as the representation of the obtained analytical data in the form of the frequencies of occurrence of particles of certain chemical or morphological class within the whole population of particles revealed in a specimen. On this basis, there were established relationships between the chemical and morphological properties of populations of particles and factors, such as the type of ammunition, the distance from the gun muzzle to the target, the type of a substrate the particles sediment on, and the time between shooting and collecting the specimens. Each of these aspects of examinations of particles revealed a great potential of being utilised in casework, while establishing various circumstances of shooting incidents leads to the reconstruction of the course of the studied incident. PMID:25025050

Molecular structure, spectral studies, NBO, HOMO-LUMO profile, MEP and Mulliken analysis of 3β,6β-dichloro-5α-hydroxy-5α-cholestane

NASA Astrophysics Data System (ADS)

Alam, Mahboob; Park, Soonheum

2018-05-01

The synthesis of 3β,6β-dichloro-5α-hydroxy-5α-cholestane (in general, steroidal chlorohydrin or steroidal halohydrin) and theoretical study of the structure are reported in this paper. The individuality of chlorohydrin was confirmed by FT-IR, NMR, MS, CHN microanalysis and X-ray crystallography. DFT calculations on the titled molecule have been performed. The molecular structure and spectra explained by Gaussian hybrid computational analysis theory (B3LYP) are found to be in correlation with the experimental data obtained from the various spectrophotometric techniques. The theoretical geometry optimization data were compared with the X-ray data. The vibrational bands appearing in the FT-IR are assigned with accuracy using harmonic frequencies along with intensities and animated modes. Molecular properties like NBO, HOMO-LUMO analysis, chemical reactivity descriptors, MEP mapping and dipole moment have been dealt at same level of theory. The calculated electronic spectrum of chlorohydrin is interpreted on the basis of TD-DFT calculations.

Curved crystal x-ray optics for monochromatic imaging with a clinical source.

PubMed

Bingölbali, Ayhan; MacDonald, C A

2009-04-01

Monochromatic x-ray imaging has been shown to increase contrast and reduce dose relative to conventional broadband imaging. However, clinical sources with very narrow energy bandwidth tend to have limited intensity and field of view. In this study, focused fan beam monochromatic radiation was obtained using doubly curved monochromator crystals. While these optics have been in use for microanalysis at synchrotron facilities for some time, this work is the first investigation of the potential application of curved crystal optics to clinical sources for medical imaging. The optics could be used with a variety of clinical sources for monochromatic slot scan imaging. The intensity was assessed and the resolution of the focused beam was measured using a knife-edge technique. A simulation model was developed and comparisons to the measured resolution were performed to verify the accuracy of the simulation to predict resolution for different conventional sources. A simple geometrical calculation was also developed. The measured, simulated, and calculated resolutions agreed well. Adequate resolution and intensity for mammography were predicted for appropriate source/optic combinations.

Recent advances in X-ray microanalysis in dermatology

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

Forslind, B.; Grundin, T.G.; Lindberg, M.

1985-01-01

Electron microprobe and proton microprobe X-ray analysis can be used in several areas of dermatological research. With a proton probe, the distribution of trace elements in human hair can be determined. Electron microprobe analysis on freeze-dried cryosections of guinea-pig and human epidermis shows a marked gradient of Na, P and K over the stratum granulosum. In sections of freeze-substituted human skin this gradient is less steep. This difference is likely to be due to a decrease in water content of the epidermis towards the stratum corneum. Electron microprobe analysis of the epidermis can, for analysis of trace elements, be complementedmore » by the proton microprobe. Quantitative agreement between the two techniques can be obtained by the use of a standard. Proton microprobe analysis was used to determine the distribution of Ni or Cr in human epidermis exposed to nickel or chromate ions. Possible differences in water content between the stratum corneum of patients with atopic eczema and normal stratum corneum was investigated in skin freeze-substituted with Br-doped resin. No significant differences were observed.« less

A Comparison of Experimental EPMA Data and Monte Carlo Simulations

NASA Technical Reports Server (NTRS)

Carpenter, P. K.

2004-01-01

Monte Carlo (MC) modeling shows excellent prospects for simulating electron scattering and x-ray emission from complex geometries, and can be compared to experimental measurements using electron-probe microanalysis (EPMA) and phi(rho z) correction algorithms. Experimental EPMA measurements made on NIST SRM 481 (AgAu) and 482 (CuAu) alloys, at a range of accelerating potential and instrument take-off angles, represent a formal microanalysis data set that has been used to develop phi(rho z) correction algorithms. The accuracy of MC calculations obtained using the NIST, WinCasino, WinXray, and Penelope MC packages will be evaluated relative to these experimental data. There is additional information contained in the extended abstract.

Cysticercosis of the fallopian tube: histology and microanalysis

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

Abraham, J.L.; Spore, W.W.; Benirschke, K.

1982-07-01

The authors identified a degenerated, focally calcified cestode larva (cysticercus) in the fallopian tube of a 50-year-old woman with endometriosis. The physiologic reaction to the larva was minimal, with some focal granulomatous salpingitis. No other focus of infection was detected. The differential diagnosis included trophoblastic tissue, foreign material, and parasites. Scanning electron microscopy and x-ray microanalysis of the organism revealed concentration of iodine in the subcuticular connective tissue of the larva and confirmed the calcium phosphate composition of the calcareous corpuscles. The presumed source of the iodine was the continued exposure of the larva to an environment rich in iodidemore » secreted by the epithelium of the fallopian tube.« less

X-ray micro-analysis of the mineralization patterns in developing enamel in hamster tooth germs exposed to fluoride in vitro during the secretory phase of amelogenesis

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

Lyaruu, D.M.; Blijleven, N.; Hoeben-Schornagel, K.

1989-09-01

The developing enamel from three-day-old hamster first maxillary (M1) molar tooth germs exposed to fluoride (F-) in vitro was analyzed for its mineral content by means of the energy-dispersive x-ray microanalysis technique. The aim of this study was to obtain semi-quantitative data on the F(-)-induced hypermineralization patterns in the enamel and to confirm that the increase in electron density observed in micrographs of F(-)-treated enamel is indeed due to an increase in mineral content in the fluorotic enamel. The tooth germs were explanted during the early stages of secretory amelogenesis and initially cultured for 24 hr in the presence ofmore » 10 ppm F- in the culture medium. The germs were then cultured for another 24 hr without F-. In order to compare the ultrastructural results directly with the microprobe data, we used the same specimens for both investigations. The net calcium counts (measurement minus background counts) in the analyses were used as a measure of the mineral content in the enamel. The aprismatic pre-exposure enamel, deposited in vivo before the onset of culture, was the most hypermineralized region in the fluorotic enamel, i.e., it contained the highest amount of calcium measured. The degree of the F(-)-induced hypermineralization gradually decreased (but was not abolished) in the more mature regions of the enamel. The unmineralized enamel matrix secreted during the initial F- treatment in vitro mineralized during the subsequent culture without F-. The calcium content in this enamel layer was in the same order of magnitude as that recorded for the newly deposited enamel in control tooth germs cultured without F-.« less

Single-particle characterization of summertime Antarctic aerosols collected at King George Island using quantitative energy-dispersive electron probe X-ray microanalysis and attenuated total reflection Fourier transform-infrared imaging techniques.

PubMed

Maskey, Shila; Geng, Hong; Song, Young-Chul; Hwang, Heejin; Yoon, Young-Jun; Ahn, Kang-Ho; Ro, Chul-Un

2011-08-01

Single-particle characterization of Antarctic aerosols was performed to investigate the impact of marine biogenic sulfur species on the chemical compositions of sea-salt aerosols in the polar atmosphere. Quantitative energy-dispersive electron probe X-ray microanalysis was used to characterize 2900 individual particles in 10 sets of aerosol samples collected between March 12 and 16, 2009 at King Sejong Station, a Korean scientific research station located at King George Island in the Antarctic. Two size modes of particles, i.e., PM(2.5-10) and PM(1.0-2.5), were analyzed, and four types of particles were identified, with sulfur-containing sea-salt particles being the most abundant, followed by genuine sea-salt particles without sulfur species, iron-containing particles, and other species including CaCO(3)/CaMg(CO(3))(2), organic carbon, and aluminosilicates. When a sulfur-containing sea-salt particle showed an atomic concentration ratio of sulfur to sodium of >0.083 (seawater ratio), it is regarded as containing nonsea-salt sulfate (nss-SO(4)(2-)) and/or methanesulfonate (CH(3)SO(3)(-)), which was supported by attenuated total reflection Fourier transform-infrared imaging measurements. These internal mixture particles of sea-salt/CH(3)SO(3)(-)/SO(4)(2-) were very frequently encountered. As nitrate-containing particles were not encountered, and the air-masses for all of the samples originated from the Pacific Ocean (based on 5-day backward trajectories), the oxidation of dimethylsulfide (DMS) emitted from phytoplanktons in the ocean is most likely to be responsible for the formation of the mixed sea-salt/CH(3)SO(3)(-)/SO(4)(2-) particles.

Scanning Electron Microscopy and Energy-Dispersive X-Ray Microanalysis of Set CEM Cement after Application of Different Bleaching Agents.

PubMed

Samiei, Mohammad; Janani, Maryam; Vahdati, Amin; Alemzadeh, Yalda; Bahari, Mahmoud

2017-01-01

The present study evaluated the element distribution in completely set calcium-enriched mixture (CEM) cement after application of 35% carbamide peroxide, 40% hydrogen peroxide and sodium perborate as commercial bleaching agents using an energy-dispersive x-ray microanalysis (EDX) system. The surface structure was also observed using the scanning electron microscope (SEM). Twenty completely set CEM cement samples, measuring 4×4 mm 2 , were prepared in the present in vitro study and randomly divided into 4 groups based on the preparation technique as follows: the control group; 35% carbamide peroxide group in contact for 30-60 min for 4 times; 40% hydrogen peroxide group with contact time of 15-20 min for 3 times; and sodium perborate group, where the powder and liquid were mixed and placed on CEM cement surface 4 times. Data were analyzed at a significance level of 0.05 through the one Way ANOVA and Tukey's post hoc tests. EDX showed similar element distribution of oxygen, sodium, calcium and carbon in CEM cement with the use of carbamide peroxide and hydroxide peroxide; however, the distribution of silicon was different ( P <0.05). In addition, these bleaching agents resulted in significantly higher levels of oxygen and carbon ( P <0.05) and a lower level of calcium ( P <0.05) compared to the control group. SEM of the control group showed plate-like and globular structure. Sodium perborate was similar to control group due to its weak oxidizing properties. Globular structures and numerous woodpecker holes were observed on the even surface on the carbamide peroxide group. The mean elemental distribution of completely set CEM cement was different when exposed to sodium perborate, carbamide peroxide and hydrogen peroxide.

Spectrum simulation in DTSA-II.

PubMed

Ritchie, Nicholas W M

2009-10-01

Spectrum simulation is a useful practical and pedagogical tool. Particularly with complex samples or trace constituents, a simulation can help to understand the limits of the technique and the instrument parameters for the optimal measurement. DTSA-II, software for electron probe microanalysis, provides both easy to use and flexible tools for simulating common and less common sample geometries and materials. Analytical models based on (rhoz) curves provide quick simulations of simple samples. Monte Carlo models based on electron and X-ray transport provide more sophisticated models of arbitrarily complex samples. DTSA-II provides a broad range of simulation tools in a framework with many different interchangeable physical models. In addition, DTSA-II provides tools for visualizing, comparing, manipulating, and quantifying simulated and measured spectra.

Size-controlled synthesis of nanocrystalline CdSe thin films by inert gas condensation

NASA Astrophysics Data System (ADS)

Sharma, Jeewan; Singh, Randhir; Kumar, Akshay; Singh, Tejbir; Agrawal, Paras; Thakur, Anup

2018-02-01

Size, shape and structure are considered to have significant influence on various properties of semiconducting nanomaterials. Different properties of these materials can be tailored by controlling the size. Size-controlled CdSe crystallites ranging from ˜ 04 to 95 nm were deposited by inert gas-condensation technique (IGC). In IGC method, by controlling the inert gas pressure in the condensation chamber and the substrate temperature or both, it was possible to produce nanoparticles with desired size. Structure and crystallite size of CdSe thin films were determined from Hall-Williamson method using X-ray diffraction data. The composition of CdSe samples was estimated by X-ray microanalysis. It was confirmed that CdSe thin film with different nanometer range crystallite sizes were synthesized with this technique, depending upon the synthesis conditions. The phase of deposited CdSe thin films also depend upon deposition conditions and cubic to hexagonal phase transition was observed with increase in substrate temperature. The effect of crystallite size on optical and electrical properties of these films was also studied. The crystallite size affects the optical band gap, electrical conductivity and mobility activation of nanocrystalline CdSe thin films. Mobility activation study suggested that there is a quasi-continuous linear distribution of three different trap levels below the conduction band.

Flux growth of high-quality CoFe 2O 4 single crystals and their characterization

NASA Astrophysics Data System (ADS)

Wang, W. H.; Ren, X.

2006-04-01

We report the growth of high-quality CoFe 2O 4 single crystals using a borax flux method. The crystals were characterized by powder X-ray diffraction, electron probe microanalysis and Raman spectroscopy. We found the crystals are flux-free and highly homogeneous in composition. X-ray rocking curves of the CoFe 2O 4 single crystals showed a full-width at half-maximum of 0.15°. The saturation magnetization of the CoFe 2O 4 single crystals was measured to be 90 emu/g or equivalently 3.65 μ B/f.u. at 5 K.

Non-destructive trace element microanalysis of as-received cometary nucleus samples using synchrotron x ray fluorescence

NASA Technical Reports Server (NTRS)

Sutton, S. R.

1989-01-01

The Synchrotron X ray Fluorescence (SXRF) microprobe at the National Synchrotron Light Source (NSLS), Brookhaven National Laboratory, will be an excellent instrument for non-destructive trace element analyses of cometary nucleus samples. Trace element analyses of as-received cometary nucleus material will also be possible with this technique. Bulk analysis of relatively volatile elements will be important in establishing comet formation conditions. However, as demonstrated for meteorites, microanalyses of individual phases in their petrographic context are crucial in defining the histories of particular components in unequilibrated specimens. Perhaps most informative in comparing cometary material with meteorites will be the halogens and trace metals. In-situ, high spatial resolution microanalyses will be essential in establishing host phases for these elements and identifying terrestrial (collection/processing) overprints. The present SXRF microprobe is a simple, yet powerful, instrument in which specimens are excited with filtered, continuum synchrotron radiation from a bending magnet on a 2.5 GeV electron storage ring. A refrigerated cell will be constructed to permit analyses at low temperatures. The cell will consist essentially of an air tight housing with a cold stage. Kapton windows will be used to allow the incident synchrotron beam to enter the cell and fluorescent x rays to exit it. The cell will be either under vacuum or continuous purge by ultrapure helium during analyses. Several other improvements of the NSLS microprobe will be made prior to the cometary nucleus sample return mission that will greatly enhance the sensitivity of the technique.

Characterization of the calcification of cardiac valve bioprostheses by environmental scanning electron microscopy and vibrational spectroscopy.

PubMed

Delogne, Christophe; Lawford, Patricia V; Habesch, Steven M; Carolan, Vikki A

2007-10-01

Bioprosthetic heart valve tissue and associated calcification were studied in their natural state, using environmental scanning electron microscopy (ESEM). Energy dispersive X-ray micro-analysis, X-ray diffraction, Fourier-transform infrared and Raman spectroscopy were used to characterize the various calcific deposits observed with ESEM. The major elements present in calcified valves were also analyzed by inductively coupled plasma-optical emission spectroscopy. To better understand the precursor formation of the calcific deposits, results from the elemental analyses were statistically correlated. ESEM revealed the presence of four broad types of calcium phosphate crystal morphology. In addition, two main patterns of organization of calcific deposits were observed associated with the collagen fibres. Energy dispersive X-ray micro-analysis identified the crystals observed by ESEM as salts containing mainly calcium and phosphate with ratios from 1.340 (possibly octacalcium phosphate, which has a Ca/P ratio of 1.336) to 2.045 (possibly hydroxyapatite with incorporation of carbonate and metal ion contaminants, such as silicon and magnesium, in the crystal lattice). Raman and fourier-transform infrared spectroscopy also identified the presence of carbonate and the analyses showed spectral features very similar to a crystalline hydroxyapatite spectrum, also refuting the presence of precursor phases such as beta-tricalcium phosphate, octacalcium phosphate and dicalcium phosphate dihydrate. The results of this study raised the possibility of the presence of precursor phases associated with the early stages of calcification.

Iron speciation of airborne subway particles by the combined use of energy dispersive electron probe X-ray microanalysis and Raman microspectrometry.

PubMed

Eom, Hyo-Jin; Jung, Hae-Jin; Sobanska, Sophie; Chung, Sang-Gwi; Son, Youn-Suk; Kim, Jo-Chun; Sunwoo, Young; Ro, Chul-Un

2013-11-05

Quantitative energy-dispersive electron probe X-ray microanalysis (ED-EPMA), known as low-Z particle EPMA, and Raman microspectrometry (RMS) were applied in combination for an analysis of the iron species in airborne PM10 particles collected in underground subway tunnels. Iron species have been reported to be a major chemical species in underground subway particles generated mainly from mechanical wear and friction processes. In particular, iron-containing particles in subway tunnels are expected to be generated with minimal outdoor influence on the particle composition. Because iron-containing particles have different toxicity and magnetic properties depending on their oxidation states, it is important to determine the iron species of underground subway particles in the context of both indoor public health and control measures. A recently developed analytical methodology, i.e., the combined use of low-Z particle EPMA and RMS, was used to identify the chemical species of the same individual subway particles on a single particle basis, and the bulk iron compositions of airborne subway particles were also analyzed by X-ray diffraction. The majority of airborne subway particles collected in the underground tunnels were found to be magnetite, hematite, and iron metal. All the particles collected in the tunnels of underground subway stations were attracted to permanent magnets due mainly to the almost ubiquitous ferrimagnetic magnetite, indicating that airborne subway particles can be removed using magnets as a control measure.

Application of a novel combination of near-infrared spectroscopy and a humidity-controlled 96-well plate to the characterization of the polymorphism of imidafenacin.

PubMed

Uchida, Hiroshi; Yoshinaga, Tokuji; Mori, Hirotoshi; Otsuka, Makoto

2010-11-01

This study aimed to apply a currently available chemometric near-infrared spectroscopy technique to the characterization of the polymorphic properties of drug candidates. The technique requires only small quantities of samples and is therefore applicable to drugs in the early stages of development. The combination of near-infrared spectroscopy and a patented 96-well plate divided into 32 individual, humidity-controlled, three-well compartments was used in the characterization of a hygroscopic drug, imidafenacin, which has two polymorphs and one pseudo-polymorph. Characterization was also conducted with powder X-ray diffraction and thermal analysis. The results were compared with those from routinely used conventional analyses. Both the microanalysis and conventional analysis successfully characterised the substance (transformation and relative stability among the two polymorphs and a pseudo-polymorph) depending on the storage conditions. Near-infrared spectroscopic analyses utilizing a humidity-controlled 96-well plate required only small amounts of the sample for characterization under the various conditions of relative humidity. Near-infrared microanalysis can be applied to polymorphic studies of small quantities of a drug candidate. The results also suggest that the method will predict the behaviors of a hygroscopic candidate in solid pharmaceutical preparations at the early stages of drug development. © 2010 The Authors. JPP © 2010 Royal Pharmaceutical Society of Great Britain.

Energy-Dispersive Spectrometry from Then until Now: A Chronology of Innovation

NASA Astrophysics Data System (ADS)

Friel, John J.; Mott, Richard B.

1998-11-01

: As part of the Microbeam Analysis Society (MAS) symposium marking 30 years of energy-dispersive spectrometry (EDS), this article reviews many innovations in the field over those years. Innovations that added a capability previously not available to the microanalyst are chosen for further description. Included are innovations in both X-ray microanalysis and digital imaging using the EDS analyzer.

Hygroscopic properties of internally mixed particles composed of NaCl and water-soluble organic acids.

PubMed

Ghorai, Suman; Wang, Bingbing; Tivanski, Alexei; Laskin, Alexander

2014-02-18

Atmospheric aging of naturally emitted marine aerosol often leads to formation of internally mixed particles composed of sea salts and water-soluble organic compounds of anthropogenic origin. Mixing of sea salt and organic components has profound effects on the evolving chemical composition and hygroscopic properties of the resulted particles, which are poorly understood. Here, we have studied chemical composition and hygroscopic properties of laboratory generated NaCl particles mixed with malonic acid (MA) and glutaric acid (GA) at different molar ratios using micro-FTIR spectroscopy, atomic force microscopy, and X-ray elemental microanalysis. Hygroscopic properties of internally mixed NaCl and organic acid particles were distinctly different from pure components and varied significantly with the type and amount of organic compound present. Experimental results were in a good agreement with the AIM modeling calculations of gas/liquid/solid partitioning in studied systems. X-ray elemental microanalysis of particles showed that Cl/Na ratio decreased with increasing organic acid component in the particles with MA yielding lower ratios relative to GA. We attribute the depletion of chloride to the formation of sodium malonate and sodium glutarate salts resulted by HCl evaporation from dehydrating particles.

Resistance in mango against infection by Ceratocystis fimbriata.

PubMed

Araujo, Leonardo; Bispo, Wilka Messner Silva; Cacique, Isaías Severino; Moreira, Wiler Ribas; Rodrigues, Fabrício Ávila

2014-08-01

This study was designed to characterize and describe host cell responses of stem tissue to mango wilt disease caused by the fungus Ceratocystis fimbriata in Brazil. Disease progress was followed, through time, in inoculated stems for two cultivars, 'Ubá' (field resistant) and 'Haden' (field susceptible). Stem sections from inoculated areas were examined using fluorescence light microscopy and transmission and scanning electron microscopy, coupled with energy-dispersive X-ray microanalysis. Tissues from Ubá colonized by C. fimbriata had stronger autofluorescence than those from Haden. The X-ray microanalysis revealed that the tissues of Ubá had higher levels of insoluble sulfur and calcium than those of Haden. Scanning electron microscopy revealed that fungal hyphae, chlamydospores (aleurioconidia), and perithecia-like structures of C. fimbriata were more abundant in Haden relative to Ubá. At the ultrastructural level, pathogen hyphae had grown into the degraded walls of parenchyma, fiber cells, and xylem vessels in the tissue of Haden. However, in Ubá, plant cell walls were rarely degraded and hyphae were often surrounded by dense, amorphous granular materials and hyphae appeared to have died. Taken together, the results of this study characterize the susceptible and resistant basal cell responses of mango stem tissue to infection by C. fimbriata.

Hygroscopic Properties of Internally Mixed Particles Composed of NaCl and Water-Soluble Organic Acids

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

Ghorai, Suman; Wang, Bingbing; Tivanski, Alexei V.

Atmospheric aging of naturally emitted marine aerosol often leads to formation of internally mixed particles composed of sea salts and water soluble organic compounds of anthropogenic origin. Mixing of sea salt and organic components has profound effects on the evolving chemical composition and hygroscopic properties of the resulted particles, which are poorly understood. Here, we have studied chemical composition and hygroscopic properties of laboratory generated NaCl particles mixed with malonic acid (MA) and glutaric acid (GA) at different molar ratios using micro-FTIR spectroscopy and X-ray elemental microanalysis.Hygroscopic properties of inte rnally mixed NaCl and organic acid particles were distinctly differentmore » from pure components and varied significantly with the type and amount of organic compound present. Experimental results were in a good agreement with the AIM modeling calculations of gas/liquid/solid partitioning in studied systems. X-ray elemental microanalysis of particles showed that Cl/Na ratio decreased with increasing organic acid component in the particles with MA yielding lower ratios relative to GA. We attribute the depletion of chloride to the formation of Na-malonate and Na-glutarate salts resulted by HCl evaporation from dehydrating particles.« less

Selective binding of Ca2+, Zn2+, Cu2+ and K+ by the physodes of the green alga Mougeotia scalaris.

PubMed

Tretyn, A; Grolig, F; Magdowski, G; Wagner, G

1996-01-01

Cells of the zygnematophycean green alga Mougeotia contain numerous globules with polyphenolic matrix, which resemble physodes. In order to analyse the capability of this compartment to sequester various ions, trichomes of Mougeotia scalaris were either fixed for X-ray microanalysis simultaneously in 2% glutardialdehyde/1% OsO4 in phosphate buffers of different K+/Na(+)-ratios, or embedded directly (fresh material) in Nanoplast resin. In addition, fixed material was treated with potassium antimonate and Ca2+ localization was examined by electron microscopic cytochemistry. A Ca(2+)-depletion upon fixation at different K+/Na(+)-ratios resulted in selective uptake of potassium, but not sodium. Consistent with earlier findings, calcium-binding by the polyphenolic physode matrix does not depend merely on electric charge but also on the presence of protonated/deprotonated phenolic groups, together with ester-linked carbonyl oxygen, which seem to be good candidates for a co-ordinate type of calcium-binding. Nanoplast embedding turned out to be the most adequate and fastest preparation for X-ray microanalysis and, apart from retaining calcium, allowed the detection of zinc and copper inside the physodes.

2D X-ray and FTIR micro-analysis of the degradation of cadmium yellow pigment in paintings of Henri Matisse

NASA Astrophysics Data System (ADS)

Pouyet, E.; Cotte, M.; Fayard, B.; Salomé, M.; Meirer, F.; Mehta, A.; Uffelman, E. S.; Hull, A.; Vanmeert, F.; Kieffer, J.; Burghammer, M.; Janssens, K.; Sette, F.; Mass, J.

2015-11-01

The chemical and physical alterations of cadmium yellow (CdS) paints in Henri Matisse's The Joy of Life (1905-1906, The Barnes Foundation) have been recognized since 2006, when a survey by portable X-ray fluorescence identified this pigment in all altered regions of the monumental painting. This alteration is visible as fading, discoloration, chalking, flaking, and spalling of several regions of light to medium yellow paint. Since that time, synchrotron radiation-based techniques including elemental and spectroscopic imaging, as well as X-ray scattering have been employed to locate and identify the alteration products observed in this and related works by Henri Matisse. This information is necessary to formulate one or multiple mechanisms for degradation of Matisse's paints from this period, and thus ensure proper environmental conditions for the storage and the display of his works. This paper focuses on 2D full-field X-ray Near Edge Structure imaging, 2D micro-X-ray Diffraction, X-ray Fluorescence, and Fourier Transform Infra-red imaging of the altered paint layers to address one of the long-standing questions about cadmium yellow alteration—the roles of cadmium carbonates and cadmium sulphates found in the altered paint layers. These compounds have often been assumed to be photo-oxidation products, but could also be residual starting reagents from an indirect wet process synthesis of CdS. The data presented here allow identifying and mapping the location of cadmium carbonates, cadmium chlorides, cadmium oxalates, cadmium sulphates, and cadmium sulphides in thin sections of altered cadmium yellow paints from The Joy of Life and Matisse's Flower Piece (1906, The Barnes Foundation). Distribution of various cadmium compounds confirms that cadmium carbonates and sulphates are photo-degradation products in The Joy of Life, whereas in Flower Piece, cadmium carbonates appear to have been a [(partially) unreacted] starting reagent for the yellow paint, a role previously suggested in other altered yellow paints.

Combined use of optical and electron microscopic techniques for the measurement of hygroscopic property, chemical composition, and morphology of individual aerosol particles.

PubMed

Ahn, Kang-Ho; Kim, Sun-Man; Jung, Hae-Jin; Lee, Mi-Jung; Eom, Hyo-Jin; Maskey, Shila; Ro, Chul-Un

2010-10-01

In this work, an analytical method for the characterization of the hygroscopic property, chemical composition, and morphology of individual aerosol particles is introduced. The method, which is based on the combined use of optical and electron microscopic techniques, is simple and easy to apply. An optical microscopic technique was used to perform the visual observation of the phase transformation and hygroscopic growth of aerosol particles on a single particle level. A quantitative energy-dispersive electron probe X-ray microanalysis, named low-Z particle EPMA, was used to perform a quantitative chemical speciation of the same individual particles after the measurement of the hygroscopic property. To validate the analytical methodology, the hygroscopic properties of artificially generated NaCl, KCl, (NH(4))(2)SO(4), and Na(2)SO(4) aerosol particles of micrometer size were investigated. The practical applicability of the analytical method for studying the hygroscopic property, chemical composition, and morphology of ambient aerosol particles is demonstrated.

The uses of synchrotron radiation sources for elemental and chemical microanalysis

USGS Publications Warehouse

Chen, J.R.; Chao, E.C.T.; Minkin, J.A.; Back, J.M.; Jones, K.W.; Rivers, M.L.; Sutton, S.R.

1990-01-01

Synchrotron radiation sources offer important features for the analysis of a material. Among these features is the ability to determine both the elemental composition of the material and the chemical state of its elements. For microscopic analysis synchrotron X-ray fluorescence (SXRF) microprobes now offer spatial resolutions of 10 ??m with minimum detection limits in the 1-10 ppm range depending on the nature of the sample and the synchrotron source used. This paper describes the properties of synchrotron radiation and their importance for elemental analysis, existing synchrotron facilities and those under construction that are optimum for SXRF microanalysis, and a number of applications including the high energy excitation of the K lines of heavy elements, microtomography, and XANES and EXAFS spectroscopies. ?? 1990.

Determination of elemental distribution in green micro-algae using synchrotron radiation nano X-ray fluorescence (SR-nXRF) and electron microscopy techniques--subcellular localization and quantitative imaging of silver and cobalt uptake by Coccomyxa actinabiotis.

PubMed

Leonardo, T; Farhi, E; Boisson, A-M; Vial, J; Cloetens, P; Bohic, S; Rivasseau, C

2014-02-01

The newly discovered unicellular micro-alga Coccomyxa actinabiotis proves to be highly radio-tolerant and strongly concentrates radionuclides, as well as large amounts of toxic metals. This study helps in the understanding of the mechanisms involved in the accumulation and detoxification of silver and cobalt. Elemental distribution inside Coccomyxa actinabiotis cells was determined using synchrotron nano X-ray fluorescence spectroscopy at the ID22 nano fluorescence imaging beamline of the European Synchrotron Radiation Facility. The high resolution and high sensitivity of this technique enabled the assessment of elemental associations and exclusions in subcellular micro-algae compartments. A quantitative treatment of the scans was implemented to yield absolute concentrations of each endogenous and exogenous element with a spatial resolution of 100 nm and compared to the macroscopic content in cobalt and silver determined using inductively coupled plasma-mass spectrometry. The nano X-ray fluorescence imaging was complemented by transmission electron microscopy coupled to X-ray microanalysis (TEM-EDS), yielding differential silver distribution in the cell wall, cytosol, nucleus, chloroplast and mitochondria with unique resolution. The analysis of endogenous elements in control cells revealed that iron had a unique distribution; zinc, potassium, manganese, molybdenum, and phosphate had their maxima co-localized in the same area; and sulfur, copper and chlorine were almost homogeneously distributed among the whole cell. The subcellular distribution and quantification of cobalt and silver in micro-alga, assessed after controlled exposure to various concentrations, revealed that exogenous metals were mainly sequestered inside the cell rather than on mucilage or the cell wall, with preferential compartmentalization. Cobalt was homogeneously distributed outside of the chloroplast. Silver was localized in the cytosol at low concentration and in the whole cell excluding the nucleus at high concentration. Exposure to low concentrations of cobalt or silver did not alter the localization nor the concentration of endogenous elements within the cells. To our knowledge, this is the first report on element co-localization and segregation at the sub-cellular level in micro-algae by means of synchrotron nano X-ray fluorescence spectroscopy.

Fabrication of luminescent SrWO{sub 4} thin films by a novel electrochemical method

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

Chen Lianping; Gao Yuanhong

2007-10-02

Highly crystallized SrWO{sub 4} thin films with single scheelite structure were prepared within 60 min by a cell electrochemical method. X-ray diffraction analysis shows that SrWO{sub 4} thin films have a tetragonal structure. Scanning electron microscopy examinations reveal that SrWO{sub 4} grains grow well in tetragonal tapers and grains like flowers or bunches, which can usually form by using the electrolysis electrochemical method, have disappeared under cell electrochemical conditions. X-ray photoelectron spectra and energy dispersive X-ray microanalysis examinations demonstrate that the composition of the film is consistent with its stoichiometry. These SrWO{sub 4} films show a single blue emission peakmore » (located at 460 nm) using an excitation wave of 230 nm. The speed of cell electrochemical method can be controlled by changing temperature. The optimum treatment temperature is about 50-60 deg. C.« less

Comparison of selective flocculation of low grade goethitic iron ore fines using natural and synthetic polymers and a graft copolymer

NASA Astrophysics Data System (ADS)

Tudu, Kichakeswari; Pal, Sagar; Mandre, N. R.

2018-05-01

This study aims to beneficiate low grade goethitic iron ore fines using a selective flocculation process. Selective flocculation studies were conducted using different polymers such as starch amylopectin (AP), poly acrylic acid (PAA), and a graft copolymer (AP-g-PAA). The obtained results were analyzed; they indicate the enhancement of the iron ore grade from 58.49% to 67.52% using AP-g-PAA with a recovery of 95.08%. In addition, 64.45% Fe with a recovery of 88.79% was obtained using AP. Similarly, using PAA, the grade increased to 63.46% Fe with a recovery of 82.10%. The findings are also supported by characterizing concentrates using X-ray diffraction (XRD) and electron probe microanalysis (EPMA) techniques.

Exploring the limits of EDS microanalysis: rare earth element analyses

NASA Astrophysics Data System (ADS)

Ritchie, N. W. M.; Newbury, D. E.; Lowers, H.; Mengason, M.

2018-01-01

It is a great time to be a microanalyst. After a few decades of incremental progress in energy-dispersive X-ray spectrometry (EDS), the last decade has seen the accuracy and precision surge forward. Today, the question is not whether EDS is generally useful but to identify the types of problems for which wavelength-dispersive X-ray spectrometry remains the better choice. The full extent of EDS’s capabilities has surprised many. Low Z, low energy, and trace element detection have been demonstrated even in the presence of extreme peak interferences. In this paper, we will summarise the state-of-the-art and investigate a challenging problem domain, the analysis of minerals bearing multiple rare-earth elements.

Formation of multicomponent matrix metal oxide films in anodic alumina matrixes by chemical deposition

NASA Astrophysics Data System (ADS)

Gorokh, G. G.; Zakhlebayeva, A. I.; Metla, A. I.; Zhilinskiy, V. V.; Murashkevich, A. N.; Bogomazova, N. V.

2017-11-01

The metal oxide films of SnxZnyOz and SnxMoyOz systems deposited onto anodic alumina matrixes by chemical and ion layering from an aqueous solutions were characterized by scanning electron microscopy, Raman spectroscopy, electron probe X-ray microanalysis and IR spectroscopy. The obtained matrix films had reproducible composition and structure and possessed certain morphological characteristics and properties.

Nondestructive characterization of municipal-solid-waste-contaminated surface soil by energy-dispersive X-ray fluorescence and low-Z (atomic number) particle electron probe X-ray microanalysis.

PubMed

Gupta, Dhrubajyoti; Ghosh, Rita; Mitra, Ajoy K; Roy, Subinit; Sarkar, Manoranjan; Chowdhury, Subhajit; Bhowmik, Asit; Mukhopadhyay, Ujjal; Maskey, Shila; Ro, Chul-Un

2011-11-01

The long-term environmental impact of municipal solid waste (MSW) landfilling is still under investigation due to the lack of detailed characterization studies. A MSW landfill site, popularly known as Dhapa, in the eastern fringe of the metropolis of Kolkata, India, is the subject of present study. A vast area of Dhapa, adjoining the current core MSW dump site and evolving from the raw MSW dumping in the past, is presently used for the cultivation of vegetables. The inorganic chemical characteristics of the MSW-contaminated Dhapa surface soil (covering a 2-km stretch of the area) along with a natural composite (geogenic) soil sample (from a small countryside farm), for comparison, were investigated using two complementary nondestructive analytical techniques, energy-dispersive X-ray fluorescence (EDXRF) for bulk analysis and low-Z (atomic number) particle electron probe X-ray microanalysis (low-Z particle EPMA) for single-particle analysis. The bulk concentrations of K, Rb, and Zr remain almost unchanged in all the soil samples. The Dhapa soil is found to be polluted with heavy metals such as Cu, Zn, and Pb (highly elevated) and Ti, Cr, Mn, Fe, Ni, and Sr (moderately elevated), compared to the natural countryside soil. These high bulk concentration levels of heavy metals were compared with the Ecological Soil Screening Levels for these elements (U.S. Environment Protection Agency) to assess the potential risk on the immediate biotic environment. Low-Z particle EPMA results showed that the aluminosilicate-containing particles were the most abundant, followed by SiO2, CaCO3-containing, and carbonaceous particles in the Dhapa samples, whereas in the countryside sample only aluminosilicate-containing and SiO2 particles were observed. The mineral particles encountered in the countryside sample are solely of geogenic origin, whereas those from the Dhapa samples seem to have evolved from a mixture of raw dumped MSW, urban dust, and other contributing factors such as wind, precipitation, weather patterns, farming, and water logging, resulting in their diverse chemical compositions and the abundant observation of carbonaceous species. Particles containing C and P were more abundant in the Dhapa samples than in the countryside soil sample, suggesting that MSW-contaminated soils are more fertile. However, the levels of particles containing potentially toxic heavy metals such as Cr, Mn, Ni, Cu, Zn, and/or Pb in the Dhapa samples were significant, corroborated by their high bulk concentration levels (EDXRF), causing deep concern for the immediate environment and contamination of the food chain through food crops.

Long term fine aerosol analysis by XRF and PIXE techniques in the city of Rijeka, Croatia

NASA Astrophysics Data System (ADS)

Ivošević, Tatjana; Orlić, Ivica; Radović, Iva Bogdanović

2015-11-01

The results of a long term, multi elemental XRF and PIXE analysis of fine aerosol pollution in the city of Rijeka, Croatia, are reported for the first time. The samples were collected during a seven months period (6th Aug 2013-28th Feb 2014) on thin stretched Teflon filters and analyzed by energy dispersive X-ray fluorescence (EDXRF) at the Laboratory for Elemental Micro-Analysis (LEMA), University of Rijeka and by Particle Induced X-ray Emission (PIXE) using 1.6 MeV protons at the Laboratory for Ion Beam Interactions (LIBI), Ruđer Bošković Institute, Zagreb. The newly developed micro-XRF system at LEMA provided results for 19 elements in the range from Si to Pb. The PIXE at the LIBI provided information for the same elements as well for the light elements such as Na, Mg and Al. Black carbon was determined with the Laser Integrated Plate Method (LIPM). The results were statistically evaluated by means of the positive matrix factorization (PMF). The seven major pollution sources were identified together with their relative contributions, these are: secondary sulfates, road traffic, smoke, road dust, sea spray, ship emissions and soil dust.

Determination of 200 °C Isothermal Section of Al-Ag-Ga Phase Diagram by Microanalysis, X-ray Diffraction, Hardness and Electrical Conductivity Measurements

NASA Astrophysics Data System (ADS)

Premović, Milena; Tomović, Milica; Minić, Duško; Manasijević, Dragan; Živković, Dragana; Ćosović, Vladan; Grković, Vladan; Đorđević, Aleksandar

2017-04-01

Ternary Al-Ag-Ga system at 200 °C was experimentally and thermodynamically assessed. Isothermal section was extrapolated using optimized thermodynamic parameters for constitutive binary systems. Microstructure and phase composition of the selected alloy samples were analyzed using light microscopy, scanning electron microscopy combined with energy-dispersive spectrometry and x-ray powder diffraction technique. The obtained experimental results were found to be in a close agreement with the predicted phase equilibria. Hardness and electrical conductivity of the alloy samples from four vertical sections Al-Ag80Ga20, Al-Ag60Ga40, Ag-Al80Ga20 and Ag-Al60Ga40 of the ternary Al-Ag-Ga system at 200 °C were experimentally determined using Brinell method and eddy current measurements. Additionally, hardness of the individual phases present in the microstructure of the studied alloy samples was determined using Vickers microhardness test. Based on experimentally obtained results, isolines of Brinell hardness and electrical conductivity were calculated for the alloys from isothermal section of the ternary Al-Ag-Ga system at 200 °C.

A 500 year sediment lake record of anthropogenic and natural inputs to Windermere (English Lake District) using double-spike lead isotopes, radiochronology, and sediment microanalysis.

PubMed

Miller, Helen; Croudace, Ian W; Bull, Jonathan M; Cotterill, Carol J; Dix, Justin K; Taylor, Rex N

2014-07-01

A high-resolution record of pollution is preserved in recent sediments from Windermere, the largest lake in the English Lake District. Data derived from X-ray core scanning (validated against wavelength dispersive X-ray fluorescence), radiochronological techniques ((210)Pb and (137)Cs) and ultrahigh precision, double-spike mass spectrometry for lead isotopes are combined to decipher the anthropogenic inputs to the lake. The sediment record suggests that while most element concentrations have been stable, there has been a significant increase in lead, zinc, and copper concentrations since the 1930s. Lead isotope down-core variations identify three major contributory sources of anthropogenic (industrial) lead, comprising gasoline lead, coal combustion lead (most likely source is coal-fired steam ships), and lead derived from Carboniferous Pb-Zn mineralization (mining activities). Periods of metal workings do not correlate with peaks in heavy metals due to the trapping efficiency of up-system lakes in the catchment. Heavy metal increases could be due to flood-induced metal inwash after the cessation of mining and the weathering of bedrock in the catchment. The combination of sediment analysis techniques used provides new insights into the pollutant depositional history of Windermere and could be similarly applied to other lake systems to determine the timing and scale of anthropogenic inputs.

Role of phi cells and the endodermis under salt stress in Brassica oleracea.

PubMed

Fernandez-Garcia, N; Lopez-Perez, L; Hernandez, M; Olmos, E

2009-01-01

Phi cell layers were discovered in the 19th century in a small number of species, including members of the Brassicaceae family. A mechanical role was first suggested for this structure; however, this has never been demonstrated. The main objective of the present work was to analyse the ultrastructure of phi cells, their influence on ion movement from the cortex to the stele, and their contribution to salt stress tolerance in Brassica oleracea. Transmission electron microscopy and X-ray microanalysis studies were used to analyse the subcellular structure and distribution of ions in phi cells and the endodermis under salt stress. Ion movement was analysed using lanthanum as an apoplastic tracer. The ultrastructural results confirm that phi cells are specialized cells showing cell wall ingrowths in the inner tangential cell walls. X-ray microanalysis confirmed a build-up of sodium. Phi thickenings were lignified and lanthanum moved periplasmically at this level. To the best of our knowledge, this is the first study reporting the possible role of the phi cells as a barrier controlling the movement of ions from the cortex to the stele. Therefore, the phi cell layer and endodermis seem to be regulating ion transport in Brassica oleracea under salt stress.

Composition of nasal airway surface liquid in cystic fibrosis and other airway diseases determined by X-ray microanalysis.

PubMed

Vanthanouvong, V; Kozlova, I; Johannesson, M; Nääs, E; Nordvall, S L; Dragomir, A; Roomans, G M

2006-04-01

The ionic composition of the airway surface liquid (ASL) in healthy individuals and in patients with cystic fibrosis (CF) has been debated. Ion transport properties of the upper airway epithelium are similar to those of the lower airways and it is easier to collect nasal ASL from the nose. ASL was collected with ion exchange beads, and the elemental composition of nasal fluid was determined by X-ray microanalysis in healthy subjects, CF patients, CF heterozygotes, patients with rhinitis, and with primary ciliary dyskinesia (PCD). In healthy subjects, the ionic concentrations were approximately isotonic. In CF patients, CF heterozygotes, rhinitis, and PCD patients, [Na] and [Cl] were significantly higher compared when compared with those in controls. [K] was significantly higher in CF and PCD patients compared with that in controls. Severely affected CF patients had higher ionic concentrations in their nasal ASL than in patients with mild or moderate symptoms. Female CF patients had higher levels of Na, Cl, and K than male patients. As higher salt concentrations in the ASL are also found in other patients with airway diseases involving chronic inflammation, it appears likely that inflammation-induced epithelial damage is important in determining the ionic composition of the ASL. Copyright (c) 2006 Wiley-Liss, Inc.

Synthesis, X-ray crystallography, spectroscopic (FT-IR, 1H &13C NMR and UV), computational (DFT/B3LYP) and enzymes inhibitory studies of 7-hydroximinocholest-5-en-3-ol acetate

NASA Astrophysics Data System (ADS)

Ahmad, Faheem; Parveen, Mehtab; Alam, Mahboob; Azaz, Shaista; Malla, Ali Mohammed; Alam, Mohammad Jane; Lee, Dong-Ung; Ahmad, Shabbir

2016-07-01

The present study reports the synthesis of 7-Hydroximinocholest-5-en-3-ol acetate (syn. 3β-acetoxycholest-5-en-7-one oxime; in general, steroidal oxime). The identity of steroidal molecule was confirmed by NMR, FT-IR, MS, CHN microanalysis and X-ray crystallography. DFT calculations on the titled molecule have been performed. The molecular structure and spectra interpreted by Gaussian hybrid computational analysis theory (B3LYP) are found to be in good correlation with the experimental data obtained from the various spectrophotometric techniques. The vibrational bands appearing in the FTIR are assigned with great accuracy using harmonic frequencies along with intensities and animated modes. Molecular properties like HOMO-LUMO analysis, chemical reactivity descriptors, MEP mapping, dipole moment and natural atomic charges have been presented at the same level of theory. Moreover, the Hirshfeld analysis was carried out to ascertain the secondary interactions and associated 2D fingerprint plots. The percentages of various interactions are pictorialized by fingerprint plots of Hirshfeld surface. Steroidal oxime exhibited promising inhibitory activity against acetylcholinesterase (AChE) as compared to the reference drug, tacrine. Molecular docking was performed to introduce steroidal molecules into the X-ray crystal structures of acetylcholinesterase at the active site to find out the probable binding mode. The results of molecular docking admitted that steroidal oxime may exhibit enzyme inhibitor activity.

Effect of Homogenization on Microstructure Characteristics, Corrosion and Biocompatibility of Mg-Zn-Mn-xCa Alloys

PubMed Central

Li, Jingyuan; Lai, Huiying; Xu, Yuzhao

2018-01-01

The corrosion behaviors of Mg-2Zn-0.2Mn-xCa (denoted as MZM-xCa alloys) in homogenization state have been investigated by immersion test and electrochemical techniques in a simulated physiological condition. The microstructure features were characterized using scanning electron microscopy (SEM), X-ray diffraction (XRD), transmission electron microscopy (TEM) and electron probe microanalysis (EPMA), and the corrosion mechanism was illustrated using atomic force microscope (AFM), X-ray photoelectron spectroscopy (XPS) and confocal laser scanning microscopy (CLSM). The electrochemical and immersion test verify the MZM-0.38% Ca owns the best corrosion performance with the corrosion rate of 6.27 mm/year. Furthermore, the film layer of MZM-0.38% Ca is more compact and denser than that of others. This improvement could be associated with the combined effects of the suitable content of Zn/Ca dissolving into the α-Mg matrix and the modification of Ca-containing compounds by heat-treatment. However, the morphologies were transformed from uniform corrosion to localized pitting corrosion with Ca further addition. It could be explained that the excessive Ca addition can strengthen the nucleation driving force for the second phase formation, and the large volumes fraction of micro-galvanic present interface sites accelerate the nucleation driving force for corrosion propagation. In addition, in vitro biocompatibility tests also show the MZM-0.38% Ca was safe to bone mesenchymal stem cells (BMSCs) and was promising to be utilized as implant materials. PMID:29389894

Structural-Phase States of Fe-Cu and Fe-Ag Bimetallic Particles Produced by Electric Explosion of Two Wires

NASA Astrophysics Data System (ADS)

Lerner, M. I.; Bakina, O. V.; Pervikov, A. V.; Glazkova, E. A.; Lozhkomoev, A. S.; Vorozhtsov, A. B.

2018-05-01

X-ray phase analysis, transmission electron microscopy, and X-ray microanalysis were used to examine the structural-phase states of Fe-Cu and Fe-Ag bimetallic nanoparticles. The nanoparticles were obtained by the electric explosion of two twisted metal wires in argon atmosphere. It was demonstrated that the nanoparticles have the structure of Janus particles. Presence of the Janus particle structure in the samples indicates formation of binary melt under conditions of combined electric explosion of two wires. Phases based on supersaturated solid solutions were not found in the examined samples. The data obtained allow arguing that it is possible to achieve uniform mixing of the two-wire explosion products under the described experiment conditions.

Nanocrystalline hydroxyapatite doped with selenium oxyanions: a new material for potential biomedical applications.

PubMed

Kolmas, Joanna; Oledzka, Ewa; Sobczak, Marcin; Nałęcz-Jawecki, Grzegorz

2014-06-01

Selenium-substituted hydroxyapatites containing selenate SeO4(2-) or selenite SeO3(2-) ions were synthesized using a wet precipitation method. The selenium content was determined by atomic absorbance spectrometry. The raw, unsintered powders were also characterized using powder X-ray diffraction, middle-range FT-IR spectroscopy and transmission electron microscopy with energy-dispersive X-ray spectroscopic microanalysis. The synthesized apatites were found to be pure and nanocrystalline with a crystal size similar to that in bone mineral. The incorporation of selenium oxyanions into the crystal lattice was confirmed. The toxicity of hydroxyapatites containing selenite or selenate ions was evaluated with a protozoan assay and bacterial luminescence test. Copyright © 2014 Elsevier B.V. All rights reserved.

Structural-Phase States of Fe–Cu and Fe–Ag Bimetallic Particles Produced by Electric Explosion of Two Wires

NASA Astrophysics Data System (ADS)

Lerner, M. I.; Bakina, O. V.; Pervikov, A. V.; Glazkova, E. A.; Lozhkomoev, A. S.; Vorozhtsov, A. B.

2018-05-01

X-ray phase analysis, transmission electron microscopy, and X-ray microanalysis were used to examine the structural-phase states of Fe-Cu and Fe-Ag bimetallic nanoparticles. The nanoparticles were obtained by the electric explosion of two twisted metal wires in argon atmosphere. It was demonstrated that the nanoparticles have the structure of Janus particles. Presence of the Janus particle structure in the samples indicates formation of binary melt under conditions of combined electric explosion of two wires. Phases based on supersaturated solid solutions were not found in the examined samples. The data obtained allow arguing that it is possible to achieve uniform mixing of the two-wire explosion products under the described experiment conditions.

Biosynthesis and characterization of silver nanoparticles prepared from two novel natural precursors by facile thermal decomposition methods

NASA Astrophysics Data System (ADS)

Goudarzi, Mojgan; Mir, Noshin; Mousavi-Kamazani, Mehdi; Bagheri, Samira; Salavati-Niasari, Masoud

2016-09-01

In this work, two natural sources, including pomegranate peel extract and cochineal dye were employed for the synthesis of silver nanoparticles. The natural silver complex from pomegranate peel extract resulted in nano-sized structures through solution-phase method, but this method was not efficient for cochineal dye-silver precursor and the as-formed products were highly agglomerated. Therefore, an alternative facile solid-state approach was investigated as for both natural precursors and the results showed successful production of well-dispersed nanoparticles with narrow size distribution for cochineal dye-silver precursor. The products were characterized by X-ray diffraction (XRD), Scanning Electron Microscopy (SEM), Energy dispersive X-ray microanalysis (EDX), and Transmission Electron Microscopy (TEM).

Reduction and Smelting of Vanadium Titanomagnetite Metallized Pellets

NASA Astrophysics Data System (ADS)

Wang, Shuai; Chen, Mao; Guo, Yufeng; Jiang, Tao; Zhao, Baojun

2018-04-01

Reduction and smelting of the vanadium titanomagnetite metallized pellets have been experimentally investigated in this study. By using the high-temperature smelting, rapid quenching, and electron probe x-ray microanalysis (EPMA) technique, the effects of basicity, reaction time, and graphite reductant amount were investigated. The vanadium contents in iron alloys increase with increasing basicity, reaction time, and graphite amount, whereas the FeO and V2O3 concentrations in the liquid phase decrease with the increase of graphite amount and reaction time. Increasing the reaction time and reductant content promotes the reduction of titanium oxide, whereas the reduction of titanium oxides can be suppressed with increasing the slag basicity. Titanium carbide (TiC) was not observed in all the quenched samples under the present conditions. The experimental results and the FactSage calculations are also compared in the present study.

Space Flight Effects on Intracellular Ions in Sublingual Cells of Non-Human Primates

NASA Technical Reports Server (NTRS)

Arnaud, Sara B.; Dotsenko, R.; Fung, P.; Navidi, M.; Silver, B.; Wade, Charles E. (Technical Monitor)

1994-01-01

We have used a novel technique that quantifies minerals and electrolytes from smears of sublingual cells by x-ray microanalysis to monitor metabolic changes in bed rest subjects. Increases in intracellular calcium (Ca), phosphorus (P), and potassium (K) were characteristic of subjects whose exercise regimen was inadequate to maintain calcium metabolism. To test the effects of space flight on intracellular ions, we analyzed cells from 2-4 kg Rhesus monkeys before and after 2 weeks in space or chair restraint (CR). There were increases in sublingual cell Ca, P and K after space flight which paralleled the clinical estimates of metabolic status of the animals and exceeded the levels found during CR on R+11. Increases after 2 weeks CR were 26% in Ca, 6% in P and 29% in K. Species similarity ill responses of intracellular ions to inactivity imposed by bed rest, restraint or microgravity suggest that this innovative non-invasive technique would be a useful in-flight monitor of exercise countermeasures directed toward maintaining calcium balance.

A Novel Forensic Investigation Applied to Bone Remains Exhumed near to Quirra Interforce Firing Range.

PubMed

Roncati, Luca; Gatti, Antonietta M; Capitani, Federico; Bonacorsi, Goretta; Barbolini, Giuseppe; Maiorana, Antonio

2016-05-01

The need to implement novel techniques, able to support a causal link between exposure and pathology, has been emerged over the recent years. The application of scanning electron microscope coupled with probe X-ray microanalysis (by means of an energy-dispersive spectroscopy) has been developed by our research group for the bone remains investigation. It was aimed to testify the exposure to microsized and nanosized pollutions, due to military activities in the Quirra interforce firing range, of a Sardinian shepherd, died of acute leukemia. Metallic debris with a combustive morphology and with an oncogenic potential has been surely detected inside his bone marrow canal. This novel technique has proved to be able to bring to light a source of past exposure preserved over time within the bone marrow canal. It can be useful for postmortem analyses, delivering a new avant-garde approach to modern forensic science. © 2015 American Academy of Forensic Sciences.

Quantitative determination of low-Z elements in single atmospheric particles on boron substrates by automated scanning electron microscopy-energy-dispersive X-ray spectrometry.

PubMed

Choël, Marie; Deboudt, Karine; Osán, János; Flament, Pascal; Van Grieken, René

2005-09-01

Atmospheric aerosols consist of a complex heterogeneous mixture of particles. Single-particle analysis techniques are known to provide unique information on the size-resolved chemical composition of aerosols. A scanning electron microscope (SEM) combined with a thin-window energy-dispersive X-ray (EDX) detector enables the morphological and elemental analysis of single particles down to 0.1 microm with a detection limit of 1-10 wt %, low-Z elements included. To obtain data statistically representative of the air masses sampled, a computer-controlled procedure can be implemented in order to run hundreds of single-particle analyses (typically 1000-2000) automatically in a relatively short period of time (generally 4-8 h, depending on the setup and on the particle loading). However, automated particle analysis by SEM-EDX raises two practical challenges: the accuracy of the particle recognition and the reliability of the quantitative analysis, especially for micrometer-sized particles with low atomic number contents. Since low-Z analysis is hampered by the use of traditional polycarbonate membranes, an alternate choice of substrate is a prerequisite. In this work, boron is being studied as a promising material for particle microanalysis. As EDX is generally said to probe a volume of approximately 1 microm3, geometry effects arise from the finite size of microparticles. These particle geometry effects must be corrected by means of a robust concentration calculation procedure. Conventional quantitative methods developed for bulk samples generate elemental concentrations considerably in error when applied to microparticles. A new methodology for particle microanalysis, combining the use of boron as the substrate material and a reverse Monte Carlo quantitative program, was tested on standard particles ranging from 0.25 to 10 microm. We demonstrate that the quantitative determination of low-Z elements in microparticles is achievable and that highly accurate results can be obtained using the automatic data processing described here compared to conventional methods.

Attempt to assess the infiltration of enamel made with experimental preparation using a scanning electron microscope.

PubMed

Skucha-Nowak, Małgorzata

2015-01-01

The resin infiltration technique, a minimally invasive method, involves the saturation, strengthening, and stabilization of demineralized enamel by a mixture of polymer resins without the need to use rotary tools or the risk of losing healthy tooth structures. To design and synthesize an experimental infiltrant with potential bacteriostatic properties.To compare the depth of infiltration of the designed experimental preparation with the infiltrant available in the market using a scanning electron microscope. Composition of the experimental infiltrant was established after analysis of 1H NMR spectra of the commercially available compounds that can penetrate pores of demineralized enamel. As the infiltrant should have bacteriostatic features by definition, an addition of 1% of monomer containing metronidazole was made. Thirty extracted human teeth were soaked in an acidic solution, which was to provide appropriate conditions for demineralization of enamel. Afterward, each tooth was divided along the coronal-root axis into two zones. One zone had experimental preparation applied to it (the test group), while the other had commercially available Icon (the control group). The teeth were dissected along the long axis and described above underwent initial observation with use of a Hitachi S-4200 scanning electron microscope. It was found that all samples contained only oxygen and carbon, regardless of the concentration of additions introduced into them. The occurrence of carbon is partially because it is a component of the preparation in question and partially because of sputtering of the sample with it. Hydrogen is also a component of the preparation, as a result of its phase composition; however, it cannot be detected by the EDS method. SEM, in combination with X-ray microanalysis, does not allow one to explicitly assess the depth of penetration of infiltration preparations into enamel.In order to assess the depth of penetration of infiltration preparations with use of X-ray microanalysis, it is recommended to introduce a contrast agent that is approved for use in dental materials, such as ytterbium III fluoride.

Combining μX-ray fluorescence, μXANES and μXRD to shed light on Zn2+ cations in cartilage and meniscus calcifications.

PubMed

Dessombz, Arnaud; Nguyen, Christelle; Ea, Hang-Korng; Rouzière, Stephan; Foy, Eddy; Hannouche, Didier; Réguer, Solene; Picca, Frederic-Emmanuel; Thiaudière, Dominique; Lioté, Frédéric; Daudon, Michel; Bazin, Dominique

2013-10-01

We aimed to examine the presence of Zn, a trace element, in osteoarthritis (OA) cartilage and meniscus from patients undergoing total knee joint replacement for primary OA. We mapped Ca(2+) and Zn(2+) at the mesoscopic scale by X-ray fluorescence microanalysis (μX-ray) to determine the spatial distribution of the 2 elements in cartilage, μX-ray absorption near edge structure spectroscopy to identify the Zn species, and μX-ray diffraction to determine the chemical nature of the calcification. Fourier transform infrared spectroscopy was used to determine the chemical composition of cartilage and meniscus. Ca(2+) showed a heterogeneous spatial distribution corresponding to the calcifications within cartilage (or meniscus) or at their surface. At least 2 Zn(2+) species were present: the first may correspond to Zn embedded in protein (different Zn metalloproteins are known to prevent calcification in biological tissues), and the second may be associated with a Zn trap in or at the surface of the calcification. Calcification present in OA cartilage may significantly modify the spatial distribution of Zn; part of the Zn may be trapped in the calcification and may alter the associated biological function of Zn metalloproteins. Copyright © 2013 Elsevier GmbH. All rights reserved.

Performance of a Commercial Silicon Drift Detector for X-ray Microanalysis

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

Kenik, Edward A

2008-01-01

Silicon drift detectors (SDDs) are rapidly becoming the energy dispersive spectrometer of choice especially for scanning electron microscopy applications. The complementary features of large active areas (i.e., collection angle) and high count rate capability of these detector contribute to their popularity, as well as the absence of liquid nitrogen cooling of the detector. The performance of an EDAX Apollo 40 SDD on a JEOL 6500F SEM will be discussed.

The concept of the phases ratio control during the formation of composite filamentary nanocrystals xInSe-(1-x)In2O3 on glass substrates

NASA Astrophysics Data System (ADS)

Gasanly, S. A.; Tomaev, V. V.; Stoyanova, T. V.

2017-11-01

The method of vacuum deposition on substrates of glass marks the C-29 series PbSe deposited film and the film In the area 3x3 mm2 and a thickness of ˜1 μm. Films are oxidized in dry air at a temperature of 550 °C. Based on studies by X-ray microanalysis and scanning electron microscopy shows the principal possibility of formation of nanowires xInSe-(1-x)In2O3 on the PbSe/In structure. The results allowed to formulate the concept of the control of phases ratio in the forming nanowires xInSe-(1-x)In2O3 on glass substrates.

Advanced microscopy of star-shaped gold nanoparticles and their adsorption-uptake by macrophages

PubMed Central

Plascencia-Villa, Germán; Bahena, Daniel; Rodríguez, Annette R.; Ponce, Arturo; José-Yacamán, Miguel

2013-01-01

Metallic nanoparticles have diverse applications in biomedicine, as diagnostics, image contrast agents, nanosensors and drug delivery systems. Anisotropic metallic nanoparticles possess potential applications in cell imaging and therapy+diagnostics (theranostics), but controlled synthesis and growth of these anisotropic or branched nanostructures has been challenging and usually require use of high concentrations of surfactants. Star-shaped gold nanoparticles were synthesized in high yield through a seed mediated route using HEPES as a precise shape-directing capping agent. Characterization was performed using advanced electron microscopy techniques including atomic resolution TEM, obtaining a detailed characterization of nanostructure and atomic arrangement. Spectroscopy techniques showed that particles have narrow size distribution, monodispersity and high colloidal stability, with absorbance into NIR region and high efficiency for SERS applications. Gold nanostars showed to be biocompatible and efficiently adsorbed and internalized by macrophages, as revealed by advanced FE-SEM and backscattered electron imaging techniques of complete unstained uncoated cells. Additionally, low voltage STEM and X-ray microanalysis revealed the ultra-structural location and confirmed stability of nanoparticles after endocytosis with high spatial resolution. PMID:23443314

PREFACE: 22nd International Congress on X-Ray Optics and Microanalysis

NASA Astrophysics Data System (ADS)

Falkenberg, Gerald; Schroer, Christian G.

2014-04-01

ICXOM22 The 22nd edition of the International Congress on X-ray Optics and Microanalysis (ICXOM 22) was held from 2-6 September 2013, in Hamburg, Germany. The congress was organized by scientists from DESY in collaboration with TU Dresden and Helmholtz-Zentrum Geesthacht, who also formed the scientific advisory board. The congress was hosted in the historical lecture hall building of the University of Hamburg located in the city center. ICXOM22 was attended by about 210 registered participants, including 67 students, and was open for listeners. The attendance was split between 26 countries (Germany 120, rest of Europe 57, America 20, Asia 8, Australia 6). The ICXOM series is a forum for the discussion of new developments in instrumentation, methods and applications in the fields of micro- and nano-analysis by means of X-ray beams. Following the trend of the last 10 years, the conference focusses more and more on synchrotron radiation rather than X-ray laboratory sources. Besides micro-beam X-ray fluorescence and absorption spectroscopy, different methods based on diffraction and full-field imaging were covered. Newly introduced to the ICXOM series was scanning coherent X-ray diffraction imaging, which was shown to evolve into a mature method for the imaging of nanostructures, defects and strain fields. New developments on fast X-ray detectors were discussed (Lambda, Maia) and advances in X-ray optics — like the generation of a sub 5nm point focus by Multilayer Zone plates — were presented. Talks on micro- and nano-analysis applications were distributed in special sessions on bio-imaging, Earth and environmental sciences, and Cultural heritage. The congress featured nine keynote and ten plenary talks, 56 talks in 14 parallel sessions and about 120 posters in three afternoon sessions. Seventeen commercial exhibitors exposed related X-ray instrumentation products, and two luncheon seminars on detector electronics were given. This allowed us to keep the student fees low and to distribute eight student travel grants. The Wednesday was devoted to an outing to DESY with guided tours to PETRA III and FLASH experiments and to the European XFEL construction site. A lecture was given by Henry Chapman introducing to structural imaging at X-ray free-electron lasers. Talks highlighting the current status and future of nanoanalysis at the leading synchrotron facilities APS (J Maser), ESRF (P Cloetens) and SPRing8 (Ishikawa) were given in the DESY auditorium offering other DESY scientists the opportunity to follow the talks. Participants A higher quality version of this image is available in supplementary data Further information about ICXOM22, including a detailed program and electronic abstract book, can be found on the congress website www.icxom22.de. We thank all the participants of ICXOM22, everybody who helped in the organization and are looking forward to hearing about further progress during ICXOM23, which will be organized by Brookhaven National Laboratory in Uptown, New York. Gerald Falkenberg ICXOM22 conference chair Christian Schroer ICXOM22 co-chair

Hydrogen peroxide changes in ischemic and reperfused heart. Cytochemistry and biochemical and X-ray microanalysis.

PubMed Central

Slezak, J.; Tribulova, N.; Pristacova, J.; Uhrik, B.; Thomas, T.; Khaper, N.; Kaul, N.; Singal, P. K.

1995-01-01

Active oxygen species including hydrogen peroxide (H2O2) play a major role in ischemia-reperfusion injury. In the present study, changes in myocardial H2O2 content as well as its subcellular distribution were examined in rat hearts subjected to ischemia-reperfusion. Isolated perfused rat hearts were made globally ischemic for 20 or 30 minutes and were reperfused for different durations. H2O2 content in these hearts was studied biochemically and changes were correlated with the recovery of function. These hearts were also analyzed for subcellular distribution of H2O2. Optimal conditions of tissue processing as well as incubation medium were established for reacting cerium chloride with H2O2 to form cerium perhydroxide, an insoluble electron-dense product. The chemical composition of these deposits was confirmed by x-ray micro-analysis. Global ischemia caused complete contractile failure in minutes and after 30 minutes of ischemia, these was a > 250% increase in the myocardial H2O2 content. Depressed contractile function recovery in the early phase of reperfusion was accompanied by approximately a 600% increase in the myocardial H2O2 content. Brief pre-fixation with low concentrations of glutaraldehyde, inhibition of alkaline phosphatase, glutathione peroxidase, and catalase, post-fixation but no post-osmication, and no counterstaining yielded the best cytochemical definition of H2O2. In normal hearts, extremely small amounts of cerium hydroperoxide precipitates were located on the endothelial cells. X-ray microanalysis confirmed the presence of cerium in the reaction product. Ischemia resulted in a stronger reaction, particularly on the sarcolemma as well as abluminal side of the endothelial cells; and upon reperfusion, cerium precipitate reaction at these sites was more intense. In the reperfused hearts, the reaction product also appeared within mitochondria between the cristae as well as on the myofibrils, but Z-lines were devoid of any precipitate. The data support a significant increase in myocardial H2O2 during both the phase of ischemia and the first few minutes of reperfusion. A stronger reaction on the sarcolemma and abluminal side of endothelial cells may also indicate enhanced H2O2 accumulation as well as vulnerability of these sites to oxidative stress injury. Images Figure 1 Figure 2 Figure 4 Figure 5 Figure 6 Figure 7 Figure 8 Figure 9 Figure 10 PMID:7677188

Micromorphology of sialoliths in submandibular salivary gland: a scanning electron microscope and X-ray diffraction analysis.

PubMed

Kasaboğlu, Oğuzcan; Er, Nuray; Tümer, Celal; Akkocaoğlu, Murat

2004-10-01

Sialoliths are common in the submandibular gland and its duct system. The exact cause of formation of a sialolith is still a matter of debate. The aim of this study was to analyze 6 sialoliths ultrastructurally to determine their development mechanism in the submandibular salivary glands. Six sialoliths retrieved from the hilus and duct of the submandibular salivary glands of 6 patients with sialadenitis were analyzed ultrastructurally by scanning electron microscope and x-ray diffractometer. Scanning electron microscope revealed mainly irregular, partly rudely hexagonal, needle-like and plate-shaped crystals. The cross-section from the surface to the inner part of the sialoliths showed no organic material. X-ray diffraction showed that the sialoliths were composed of hydroxyapatite crystals. Energy dispersive x-ray microanalysis showed that all of the samples contained high levels of Ca and P, and small amounts of Mg, Na, Cl, Si, Fe, and K. The main structures of the submandibular sialoliths were found to be hydroxyapatite crystals. No organic cores were observed in the central parts of the sialoliths. In accordance with these preliminary results, sialoliths in the submandibular salivary glands may arise secondary to sialadenitis, but not via a luminal organic nidus.

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

NASA Astrophysics Data System (ADS)

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

2010-06-01

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

Microanalysis study of archaeological mural samples containing Maya blue pigment

NASA Astrophysics Data System (ADS)

Sánchez del Río, M.; Martinetto, P.; Somogyi, A.; Reyes-Valerio, C.; Dooryhée, E.; Peltier, N.; Alianelli, L.; Moignard, B.; Pichon, L.; Calligaro, T.; Dran, J.-C.

2004-10-01

Elemental analysis by X-ray fluorescence and particle induced X-ray emission is applied to the study of several Mesoamerican mural samples containing blue pigments. The most characteristic blue pigment is Maya blue, a very stable organo-clay complex original from Maya culture and widely used in murals, pottery and sculptures in a vast region of Mesoamerica during the pre-hispanic time (from VIII century) and during the colonization until 1580. The mural samples come from six different archaeological sites (four pre-hispanic and two from XVI century colonial convents). The correlation between the presence of some elements and the pigment colour is discussed. From the comparative study of the elemental concentration, some conclusions are drawn on the nature of the pigments and the technology used.

Hair casts due to a deodorant spray.

PubMed

Ena, Pasquale; Mazzarello, Vittorio; Chiarolini, Fausto

2005-11-01

A 7-year-old girl presented with itching and greyish-white sleeve-like structures in her hair. After ruling out other possible causes for the symptoms, such as nits and dandruff, it was determined that the patient was affected by hair casts. These are small cylindrical structures resembling louse eggs that encircle individual scalp hairs and are easily movable along the hair shafts. It was concluded that she had induced the condition through misuse of a deodorant body spray. Scanning electron microscopy combined with electron dispersive X-ray analysis (X-ray microanalysis) of the hair casts showed the chemical nature of the structures. Some elements present in the composition of the ingredients of the deodorant spray, such as aluminium, chlorine, silicon, magnesium and carbon, were also present in this uncommon type of hair casts.

THE WEATHERING OF A SULFIDE OREBODY: SPECIATION AND FATE OF SOME POTENTIAL CONTAMINANTS

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

Courtin-Nomade, Alexandra; Grosbois, Cecile; Marcus, Matthew A.

2010-07-16

Various potentially toxic trace elements such as As, Cu, Pb and Zn have been remobilized by the weathering of a sulfide orebody that was only partially mined at Leona Heights, California. As a result, this body has both natural and anthropogenically modified weathering profiles only 500 m apart. The orebody is located in a heavily urbanized area in suburban Oakland, and directly affects water quality in at least one stream by producing acidic conditions and relatively high concentrations of dissolved elements (e.g., {approx}500 mg/L Cu, {approx}3700 mg/L Zn). Micrometric-scale mineralogical investigations were performed on the authigenic metal-bearing phases (less thanmore » 10 {mu}m in size) using electron-probe micro-analysis (EPMA), micro-Raman, micro X-ray absorption spectroscopy (mXAS), scanning X-ray diffraction (mSXRD) and scanning X-ray fluorescence (mSXRF) mapping techniques. Those measurements were coupled with classical mineralogical laboratory techniques, X-ray diffraction (XRD) and scanning electron microscopy (SEM). Authigenic metal-bearing phases identified are mainly sulfates (jarosite, epsomite, schwertmannite), Fe (oxy-)hydroxides (goethite, hematite and poorly crystalline Fe products) and poorly crystalline Mn (hydr-)oxides. Sulfates and Fe (oxy-)hydroxides are the two main secondary products at both sites, whereas Mn (hydr-) oxides were only observed in the samples from the non-mining site. In these samples, the various trace elements show different affinities for Fe or Mn compounds. Lead is preferentially associated with Mn (hydr-)oxides and As with Fe (oxy-)hydroxides or sulfates. Copper association with Mn and Fe phases is questionable, and the results obtained rather indicate that Cu is present as individual Cu-rich grains (Cu hydroxides). Some ochreous precipitates were found at both sites and correspond to a mixture of schwertmannite, goethite and jarosite containing some potentially toxic trace elements such as Cu, Pb and Zn. According to the trace element distribution and relative abundance of the unweathered sulfides, this orebody still represents a significant reservoir of potential contaminants for the watershed, especially in the non-mining site, as a much greater proportion of sulfides is left to react and because of the lower porosity in this site.« less

The weathering of a sulfide orebody: Speciation and fate of some potential contaminants

USGS Publications Warehouse

Courtin-Nomade, A.; Grosbois, C.; Marcus, M.A.; Fakra, S.C.; Beny, J.-M.; Foster, A.L.

2009-01-01

Various potentially toxic trace elements such as As, Cu, Pb and Zn have been remobilized by the weathering of a sulfide orebody that was only partially mined at Leona Heights, California. As a result, this body has both natural and anthropogeni- cally modified weathering profiles only 500 m apart. The orebody is located in a heavily urbanized area in suburban Oakland, and directly affects water quality in at least one stream by producing acidic conditions and relatively high concentrations of dissolved elements (e.g., ??500 ??g/L Cu, ??3700 ??g/L Zn). Micrometric-scale mineralogical investigations were performed on the authigenic metal-bearing phases (less than 10 ??m in size) using electron-probe micro-analysis (EPMA), micro-Raman, micro X-ray absorption spectroscopy (??XAS), scanning X-ray diffraction ((??SXRD) and scanning X-ray fluorescence (??-SXRF) mapping techniques. Those measurements were coupled with classical mineralogical laboratory techniques, X-ray diffraction (XRD) and scanning electron microscopy (SEM). Authigenic metal-bearing phases identified are mainly sulfates (jarosite, epsomite, schwertmannite), Fe (oxy-)hydroxides (goethite, hematite and poorly crystalline Fe products) and poorly crystalline Mn (hydr-)oxides. Sulfates and Fe (oxy-)hydroxides are the two main secondary products at both sites, whereas Mn (hydr-) oxides were only observed in the samples from the non-mining site. In these samples, the various trace elements show different affinities for Fe or Mn compounds. Lead is preferentially associated with Mn (hydr-)oxides and As with Fe (oxy-)hydroxides or sulfates. Copper association with Mn and Fe phases is questionable, and the results obtained rather indicate that Cu is present as individual Cu-rich grains (Cu hydroxides). Some ochreous precipitates were found at both sites and correspond to a mixture of schwertmannite, goethite and jarosite containing some potentially toxic trace elements such as Cu, Pb and Zn. According to the trace element distribution and relative abundance of the unweathered sulfides, this orebody still represents a significant reservoir of potential contaminants for the watershed, especially at the non-mining site, as a much greater proportion of sulfides is left to react and because of the lower porosity at this site.

III-Nitride Based Optoelectronics

DTIC Science & Technology

2010-01-01

carrier gas67 is known to affect the atomic composition of etched ZnO surface. In our research, we have used x- ray microanalysis to gather...Project (0704-0188.) Washington, DC 20503. 1. AGENCY USE ONLY ( Leave Blank) 2. REPORT DATE 03/2010 3. REPORT TYPE AND DATES COVERED Final...Introduction 2 2.2 Experiment 3 2.2.1 Growth and Material Characterization 3 2.2.2 Preparation of high quality LEO GaN 3 2.2.3 Blue and green active

Study of some health physics parameters of bismuth-ground granulated blast furnace slag shielding concretes

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

Kumar, Sandeep, E-mail: sandeep0078monu@gmail.com; Singh, Sukhpal, E-mail: sukhpal-78@rediffmail.com

2016-05-06

The Bismuth-ground granulated blastfurnace slang (Bi-GGBFS) concrete samples were prepared. The weight percentage of different elements present in Bi-GGBFS Shielding concretewas evaluated by Energy Dispersive X-ray Microanalysis (EDX). The exposure rate and absorbed dose rate characteristics were calculated theoretically for radioactive sources namely {sup 241}Am and {sup 137}Cs. Our calculations reveal that the Bi-GGBFS concretes are effective in shielding material for gamma radiations.

Scanning probe microscopy in mineralogical studies: about origin of the observed roughness of natural silica-rich glasses

NASA Astrophysics Data System (ADS)

Golubev, Ye A.; Isaenko, S. I.

2017-10-01

We have studied different mineralogical objects: natural glasses of impact (tektites, impactites) and volcanic (obsidians) origin, using atomic force microscopy, X-ray microanalysis, infrared and Raman spectroscopy. The spectroscopy showed the difference in the structure and chemical composition of the glasses of different origin. The analysis of the dependence of nanoscale heterogeneity of the glasses, revealed by the atomic force microscopy, on their structural and chemical features was carried out.

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

Vilches, J.; Lopez, A.; Martinez, M.C.

This paper discusses the value of scanning electron microscopy (SEM) and x-ray microanalysis in the classification of craniopharyngiomas. This neoplasm shows epithelial nest, cords of cuboid cells, foci of squamous metaplasia, and microcystic degeneration. SEM reveals that the epithelial cysts are lined with elongated cells that possess numerous microvilli and blebs and that some cysts are lined with polyhedral cells. The microvilli are interpreted as characteristic of the fast growing craniopharyngiomas. A microanalytical study of the calcified areas reveals the presence of magnesium, phosphorus, and calcium.

Correlative Instrumental Neutron Activation Analysis, Light Microscopy, Transmission Electron Microscopy, and X-ray Microanalysis for Qualitative and Quantitative Detection of Colloidal Gold Spheres in Biological Specimens

NASA Astrophysics Data System (ADS)

Hillyer, Julián F.; Albrecht, Ralph M.

1998-10-01

: Colloidal gold, conjugated to ligands or antibodies, is routinely used as a label for the detection of cell structures by light (LM) and electron microscopy (EM). To date, several methods to count the number of colloidal gold labels have been employed with limited success. Instrumental neutron activation analysis (INAA), a physical method for the analysis of the elemental composition of materials, can be used to provide a quantitative index of gold accumulation in bulk specimens. Given that gold is not naturally found in biological specimens in any substantial amount and that colloidal gold and ligand conjugates can be prepared to yield uniform bead sizes, the amount of label can be calculated in bulk biological samples by INAA. Here we describe the use of INAA, LM, transmission EM, and X-ray microanalysis (EDX) in a model to determine both distribution (localization) and amount of colloidal gold at the organ, tissue, cellular, and ultrastructural levels in whole animal systems following administration. In addition, the sensitivity for gold in biological specimens by INAA is compared with that of inductively coupled plasma mass spectrometry (ICP-MS). The correlative use of INAA, LM, TEM, and EDX can be useful, for example, in the quantitative and qualitative tracking of various labeled molecular species following administration in vivo.

Abandoned mine slags analysis by EPMA WDS X-ray mapping

NASA Astrophysics Data System (ADS)

Guimarães, F.; Rosado, L.; Morais, C.; Candeias, A. E.; Pinto, A. P.; Mirão, J.

2010-02-01

Mining activity on the Iberian Pyritic Belt (Portugal and Spain) started before Phoenician times, became particularly intense during the Roman occupation of the Iberian Peninsula (for gold), and after the industrial revolution (for gold, copper, zinc, lead and sulphur). The commonest ore of this region is a massive polymetalic sulphide accumulation, where pyrite (FeS2) is the main mineral, with variable concentrations of chalcopyrite (CuFeS2), sphalerite (ZnS), galena (PbS), arsenopyrite (FeAsS2), other sulphides and sulfosalts which include minor elements like Mn, Co, Ni, Se, Cd, Sb, Te, Hg and Bi. Some of the main and minor elements of these ores are hazardous and the drainage basins of pollutant source areas often induce health concerns in the resident population. Electron probe microanalysis study followed previous optical and XRD analysis of the slags. The study focused on the identification of phases how sulphide and metallic phases are distributed within the material and infer about leachable elements during weathering. Electron probe X-ray maps show evidences of different behaviour between the elements: Ca and Zn are completely leached; iron is retained in oxyhydroxides, lead and arsenic precipitate as sulphates. Electron probe microanalysis studies are essential to understand complex materials as earth materials. Nevertheless, care is required to a correct interpretation of data and most quantitative compositional data are not trustworthy.

The osteoplastic effectiveness of the implants made of mesh titanium nickelide constructs.

PubMed

Mikhailovich Irianov, Iurii; Vladimirovna Diuriagina, Olga; Iurevna Karaseva, Tatiana; Anatolevich Karasev, Evgenii

2014-02-01

The purpose of the work was to study the features of reparative osteogenesis for filling the defect of tubular bone under implantation of mesh titanium nickelide constructs. Tibial fenestrated defect was modeled experimentally in 30 Wistar pubertal rats, followed by implant intramedullary insertion. The techniques of radiography, scanning electron microscopy and X-ray electron probe microanalysis were used. The mesh implant of titanium nickelide has been established to possess biocompatibility, osteoconductive and osteoinductive properties, the zone of osteogenesis and angiogenesis is created around it, bone cover is formed. Osteointegration of the implant occurs early, by 7 days after surgery, and by 30 days after surgery organotypical re-modelling of the regenerated bone takes place, as well as the defect is filled with lamellar bone tissue by the type of bone wound primary adhesion. By 30 days after surgery mineral content of the regenerated bone tissue approximates to the composition of intact cortex mineral phase.

Influence of mechanical and chemical surface treatments on the formation of bone-like structure in cpTi for endosseous dental implants

NASA Astrophysics Data System (ADS)

Parsikia, Farhang; Amini, Pupak; Asgari, Sirous

2012-10-01

Commercially pure titanium samples were exposed to grit blasting and acid-alkali treatments to obtain a variety of surface compositions and morphologies. Contact roughness test and microstructural studies were employed to study the surface topography of the samples. The nature and chemical composition of surface phases were evaluated using X-ray diffraction and microanalysis techniques. Selected samples first exposed to in vitro environment were then tested to determine the surface morphology and surface microstructure. Based on the data presented in this work, it is suggested that grit blasting process utilized prior to chemical treatment stage, yields a high quality surface morphology. Such a surface morphology is expected to have superior tribological characteristics after osseointegration. Also, it appeared that the reverse sequence of processing resulted in a better biocompatibility of the product manifested by negligible amount of residual alumina on the sample surface.

Thermoelectric properties of Ge 1-xSn xTe crystals grown by vertical Bridgman method

NASA Astrophysics Data System (ADS)

Wu, C. C.; Ferng, N. J.; Gau, H. J.

2007-06-01

Single crystals of Ge 1-xSn xTe compounds with x=0, 0.8, 0.9 and 1.0 were grown by vertical Bridgman method. The crystalline phase and stochiometry for these crystals were investigated by X-ray diffraction, metallographic microscope as well as electron-probe microanalysis (EPMA). Electrical property of the as-grown samples was characterized using room temperature resistivity and Hall measurements. The thermoelectric behaviors for the Ge 1-xSn xTe crystals were studied by means of thermal and carrier transport measurements. Temperature dependences of resistivity, Seebeck coefficient and thermal conductivity for the various compositions of Ge 1-xSn xTe were analyzed. A two-valence band model was proposed to describe the temperature dependence of thermoelectric property of the Ge 1-xSn xTe crystals. The dimensionless thermoelectric figure of merit ZT for the alloys was evaluated and discussed.

Electrolytic Reduction of Titania Slag in Molten Calcium Chloride Bath

NASA Astrophysics Data System (ADS)

Mohanty, Jayashree

2012-05-01

Ferro-titanium is prepared by direct electrolytic reduction of titania-rich slag obtained from plasma smelting of ilmenite in molten CaCl2. The product after electro-reduction is characterized by x-ray diffraction, scanning electron microscopy, and electron probe microanalysis. The electrolysis is carried out at a cell voltage of 3.0 V, taking graphite as the electrolysis cell as well as the anode, and a titania-rich slag piece wrapped by a nichrome wire is used as the cathode.

Properties of calcium-containing microparticles formed in the process of biomineralization of the human aortic wall

NASA Astrophysics Data System (ADS)

Zlatoustova, O. Yu; Vasilev, S. V.; Rudy, A. S.

2016-08-01

The results of the study of human aortic walls, subjected to different stages of mineralization are presented. By means of scanning electron microscopy and X-ray microanalysis the morphology, elemental composition and characteristics of the mineral component localization were investigated. The key differences in the initial, intermediate and final stages of pathological mineralization of the aorta wall were identified. The data obtained may be useful in describing the mechanism of biomineral deposits formation in human body.

[Bone defect replacement under conditions of transosseous osteosynthesis and titanium nickelide implant application].

PubMed

Ir'ianov, Iu M; Ir'ianova, T Iu

2012-01-01

In the experiment conducted on 30 Wistar rats, the peculiarities of tibial bone defect replacement under conditions of transosseous osteosynthesis and implantation of titanium nickelide mesh structures were studied using the methods of scanning electron microscopy and x-ray electron probe microanalysis. It was demonstrated that implant osseointegration occured 7 days after surgery, and after 30 days the defect was replaced with bone tissue by the type of primary bone wound healing, thus the organotypical remodeling of regenerated bone took place.

Inter-layered clay stacks in Jurassic shales

NASA Technical Reports Server (NTRS)

Pye, K.; Krinsley, D. H.

1983-01-01

Scanning electron microscopy in the backscattered electron mode is used together with energy-dispersive X-ray microanalysis to show that Lower Jurassic shales from the North Sea Basin contain large numbers of clay mineral stacks up to 150 microns in size. Polished shale sections are examined to determine the size, shape orientation, textural relationships, and internal compositional variations of the clays. Preliminary evidence that the clay stacks are authigenic, and may have formed at shallow burial depths during early diagenesis, is presented.

Structural investigation of cooperite (PtS) crystals

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

Rozhdestvina, V. I., E-mail: veronika@ascnet.ru; Udovenko, A. A.; Rubanov, S. V.

2016-03-15

The single-crystal structure of cooperite, a natural platinum sulfide PtS, is studied by X-ray diffraction supported by high-resolution scanning transmission electron microscopy and X-ray spectrum microanalysis. It is found that, in addition to the main reflections corresponding to the known tetragonal cell (a = 3.47 and c = 6.11 Å; space group P4{sub 2}/mmc), many weak reflections with intensities I ≤ 60σ(I) are clearly observed. These reflections fit the tetragonal cell (space group I4/mmm) with doubled parameters. In structures with small (P4{sub 2}/mmc) and large (I4/mmm) cells, the S atoms occupy statistically two special positions. It is shown that themore » chemical composition of the cooperite crystals deviates from the stoichiometric composition: sulfur-deficient specimens predominate.« less

Hydroxyapatite coatings produced on commercially pure titanium by micro-arc oxidation.

PubMed

Huang, Yong; Wang, Yingjun; Ning, Chengyun; Nan, Kaihui; Han, Yong

2007-09-01

A porous hydroxyapatite (HA) coating on commercially pure titanium was prepared by micro-arc oxidation (MAO) in electrolytic solution containing calcium acetate and beta-glycerol phosphate disodium salt pentahydrate (beta-GP). The thickness, phase, composition morphology and biocompatibility of the oxide coating were characterized by x-ray diffraction (XRD), electron probe microanalysis (EPMA), scanning electron microscopy (SEM) with an energy dispersive x-ray spectrometer (EDS) and cell culture. The thickness of the MAO film was about 20 microm, and the coating was porous and uneven without any apparent interface to the titanium substrates. The result of XRD showed that the porous coating was made up of HA film. The favorable osteoblast cell affinity gives HA film good biocompatibility. HA coatings are expected to have significant uses for medical applications such as dental implants and artificial bone joints.

Microstructure of In x Ga1-x N nanorods grown by molecular beam epitaxy

NASA Astrophysics Data System (ADS)

Webster, R. F.; Soundararajah, Q. Y.; Griffiths, I. J.; Cherns, D.; Novikov, S. V.; Foxon, C. T.

2015-11-01

Transmission electron microscopy is used to examine the structure and composition of In x Ga1-x N nanorods grown by plasma-assisted molecular beam epitaxy. The results confirm a core-shell structure with an In-rich core and In-poor shell resulting from axial and lateral growth sectors respectively. Atomic resolution mapping by energy-dispersive x-ray microanalysis and high angle annular dark field imaging show that both the core and the shell are decomposed into Ga-rich and In-rich platelets parallel to their respective growth surfaces. It is argued that platelet formation occurs at the surfaces, through the lateral expansion of surface steps. Studies of nanorods with graded composition show that decomposition ceases for x ≥ 0.8 and the ratio of growth rates, shell:core, decreases with increasing In concentration.

Testing a laser-induced breakdown spectroscopy technique on the Arctic sediments

NASA Astrophysics Data System (ADS)

Han, D.; Nam, S. I.

2017-12-01

Physical and geochemical investigations coupled with the Laser-induced Breakdown Spectroscopy (LIBS) were performed on three surface sediment cores (ARA03B/24BOX, ARA02B/01(A)MUC, ARA02B/02MUC and ARA02B/03(A)MUC) recovered from the western Arctic Ocean (Chukchi Sea) during IBRV ARON expeditions in 2012. The LIBS technique was applied to carry out elemental chemical analysis of the Arctic sediments and compared with that measured by ITRAX X-ray fuorescence (XRF) core scanning. LIBS and XRF have shown similar elemental composition within each sediment core. In this study, mineral composition (XRD), grain size distribution and organic carbon content as well as elemental composition (LIBS) were all considered to understand paleoenvironmental changes (ocean circulation, sea-ice drift, iceberg discharge, and etc.) recorded in the Arctic Holocene sediment. Quantitative LIBS analysis shows a gradually varying distribution of the elements along the sampled core and clear separation between the cores. The cores are geochemically characterized by elevated Mn profile. The gradient of mineral composition and grain sizes among the cores shows regional distribution and variation in sedimentary condition due to geological distance between East Siberian and North America. The present study reveals that a LIBS technique can be employed for in-situ sediment analyses for the Arctic Ocean. Furthermore, LIBS does not require costly equipment, trained operators, and complicated sample pre-treatment processes compared to Atomic absorption spectroscopy (AAS) and inductively coupled plasma emission spectroscopy (ICP), and also known to show relatively high levels of sensitivity, precision, and distinction than XRF analysis, scanning electron microscopy-energy dispersive spectrometry (SEM-EDS), and electron probe X-ray microanalysis (EPMA).

Back-bombardment compensation in microwave thermionic electron guns

NASA Astrophysics Data System (ADS)

Kowalczyk, Jeremy M. D.; Madey, John M. J.

2014-12-01

The development of capable, reliable, and cost-effective compact electron beam sources remains a long-standing objective of the efforts to develop the accelerator systems needed for on-site research and industrial applications ranging from electron beam welding to high performance x-ray and gamma ray light sources for element-resolved microanalysis and national security. The need in these applications for simplicity, reliability, and low cost has emphasized solutions compatible with the use of the long established and commercially available pulsed microwave rf sources and L-, S- or X-band linear accelerators. Thermionic microwave electron guns have proven to be one successful approach to the development of the electron sources for these systems providing high macropulse average current beams with picosecond pulse lengths and good emittance out to macropulse lengths of 4-5 microseconds. But longer macropulse lengths are now needed for use in inverse-Compton x-ray sources and other emerging applications. We describe in this paper our approach to extending the usable macropulse current and pulse length of these guns through the use of thermal diffusion to compensate for the increase in cathode surface temperature due to back-bombardment.

Plutonium-uranium mixed oxide characterization by coupling micro-X-ray diffraction and absorption investigations

NASA Astrophysics Data System (ADS)

Degueldre, C.; Martin, M.; Kuri, G.; Grolimund, D.; Borca, C.

2011-09-01

Plutonium-uranium mixed oxide (MOX) fuels are currently used in nuclear reactors. The potential differences of metal redox state and microstructural developments of the matrix before and after irradiation are commonly analysed by electron probe microanalysis. In this work the structure and next-neighbor atomic environments of Pu and U oxide features within unirradiated homogeneous MOX and irradiated (60 MW d kg -1) MOX samples was analysed by micro-X-ray fluorescence (μ-XRF), micro-X-ray diffraction (μ-XRD) and micro-X-ray absorption fine structure (μ-XAFS) spectroscopy. The grain properties, chemical bonding, valences and stoichiometry of Pu and U are determined from the experimental data gained for the unirradiated as well as for irradiated fuel material examined in the center of the fuel as well as in its peripheral zone (rim). The formation of sub-grains is observed as well as their development from the center to the rim (polygonization). In the irradiated sample Pu remains tetravalent (>95%) and no (<5%) Pu(V) or Pu(VI) can be detected while the fuel could undergo slight oxidation in the rim zone. Any slight potential plutonium oxidation is buffered by the uranium dioxide matrix while locally fuel cladding interaction could also affect the redox of the fuel.

New frontiers in water purification: highly stable amphopolycarboxyglycinate-stabilized Ag-AgCl nanocomposite and its newly discovered potential

NASA Astrophysics Data System (ADS)

Krutyakov, Yurii A.; Zherebin, Pavel M.; Kudrinskiy, Alexey A.; Zubavichus, Yan V.; Presniakov, Mikhail Yu; Yapryntsev, Alexey D.; Karabtseva, Anastasia V.; Mikhaylov, Dmitry M.; Lisichkin, Georgii V.

2016-09-01

A simple synthetic procedure for high-stable dispersions of porous composite Ag/AgCl nanoparticles stabilized with amphoteric surfactant sodium tallow amphopolycarboxyglycinate has been proposed for the first time. The prepared samples were characterized by UV-vis spectroscopy, x-ray powder diffraction (XRD), x-ray photoelectron spectroscopy, small area electron diffraction (SAED), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), and electron probe micro-analysis. In addition, measurements (carried out at the Kurchatov synchrotron radiation source stations) of the Ag K-edge extended x-ray absorption fine structure (EXAFS) and x-ray absorption near edge structure (XANES) spectra and XRD of the prepared nanoparticles have been performed. The obtained results suggest that small-sized Ag clusters are homogeneously distributed in the mass of the AgCl nanoparticle (~80 nm) formed during the synthesis. The Ag/AgCl dispersion demonstrates photocatalytic activity (with respect to methyl orange) and high bactericidal activity against E. coli. This activity is superior to the activity of both Ag and AgCl nanoparticles stabilized by the same surfactant. Thus, porous composite Ag/AgCl nanoparticles can be used as a multifunctional agent that is able to remove both pollutants and bacterium from water.

Study of the specific features of single-crystal boron microstructure

NASA Astrophysics Data System (ADS)

Blagov, A. E.; Vasil'ev, A. L.; Dmitriev, V. P.; Ivanova, A. G.; Kulikov, A. G.; Marchenkov, N. V.; Popov, P. A.; Presnyakov, M. Yu.; Prosekov, P. A.; Pisarevskii, Yu. V.; Targonskii, A. V.; Chernaya, T. S.; Chernyshov, D. Yu.

2017-09-01

A complex study of the structure of β-boron single crystal grown by the floating-zone method, with sizes significantly exceeding the analogs known in the literature, has been performed. The study includes X-ray diffraction analysis and X-ray diffractometry (measurement of pole figures and rocking curves), performed on both laboratory and synchrotron sources; atomic-resolution scanning transmission electron microscopy with spherical aberration correction; and energy-dispersive microanalysis. X-ray diffraction analysis using synchrotron radiation has been used to refine the β-boron structure and find impurity Si atoms. The relative variations in the unit-cell parameters a and c for the crystal bulk are found to be δ a/ a ≈ 0.4 and δ c/ c ≈ 0.1%. X-ray diffractometry has revealed that the single-crystal growth axis coincides with the [2\\bar 2013] crystallographic axis and makes an angle of 21.12° with the [0001] threefold axis. Electron microscopy data have confirmed that the sample under study is a β-boron crystal, which may contain 0.3-0.4 at % Si as an impurity. Planar defects (stacking faults and dislocations) are found. The results of additional measurements of the temperature dependence of the thermal conductivity of the crystal in the range of 50-300 K are indicative of its high structural quality.

Complementary Characterization of Cu(In,Ga)Se₂ Thin-Film Photovoltaic Cells Using Secondary Ion Mass Spectrometry, Auger Electron Spectroscopy, and Atom Probe Tomography.

PubMed

Jang, Yun Jung; Lee, Jihye; Jeong, Jeung-Hyun; Lee, Kang-Bong; Kim, Donghwan; Lee, Yeonhee

2018-05-01

To enhance the conversion performance of solar cells, a quantitative and depth-resolved elemental analysis of photovoltaic thin films is required. In this study, we determined the average concentration of the major elements (Cu, In, Ga, and Se) in fabricated Cu(In,Ga)Se2 (CIGS) thin films, using inductively coupled plasma atomic emission spectroscopy, X-ray fluorescence, and wavelengthdispersive electron probe microanalysis. Depth profiling results for CIGS thin films with different cell efficiencies were obtained using secondary ion mass spectrometry and Auger electron spectroscopy to compare the atomic concentrations. Atom probe tomography, a characterization technique with sub-nanometer resolution, was used to obtain three-dimensional elemental mapping and the compositional distribution at the grain boundaries (GBs). GBs are identified by Na increment accompanied by Cu depletion and In enrichment. Segregation of Na atoms along the GB had a beneficial effect on cell performance. Comparative analyses of different CIGS absorber layers using various analytical techniques provide us with understanding of the compositional distributions and structures of high efficiency CIGS thin films in solar cells.

HA/nylon 6,6 porous scaffolds fabricated by salt-leaching/solvent casting technique: effect of nano-sized filler content on scaffold properties

PubMed Central

Mehrabanian, Mehran; Nasr-Esfahani, Mojtaba

2011-01-01

Nanohydroxyapatite (n-HA)/nylon 6,6 composite scaffolds were produced by means of the salt-leaching/solvent casting technique. NaCl with a distinct range size was used with the aim of optimizing the pore network. Composite powders with different n-HA contents (40%, 60%) for scaffold fabrication were synthesized and tested. The composite scaffolds thus obtained were characterized for their microstructure, mechanical stability and strength, and bioactivity. The microstructure of the composite scaffolds possessed a well-developed interconnected porosity with approximate optimal pore size ranging from 200 to 500 μm, ideal for bone regeneration and vascularization. The mechanical properties of the composite scaffolds were evaluated by compressive strength and modulus tests, and the results confirmed their similarity to cortical bone. To characterize bioactivity, the composite scaffolds were immersed in simulated body fluid for different lengths of time and results monitored by scanning electron microscopy and energy dispersive X-ray microanalysis to determine formation of an apatite layer on the scaffold surface. PMID:21904455

Combined use of quantitative ED-EPMA, Raman microspectrometry, and ATR-FTIR imaging techniques for the analysis of individual particles.

PubMed

Jung, Hae-Jin; Eom, Hyo-Jin; Kang, Hyun-Woo; Moreau, Myriam; Sobanska, Sophie; Ro, Chul-Un

2014-08-21

In this work, quantitative energy-dispersive electron probe X-ray microanalysis (ED-EPMA) (called low-Z particle EPMA), Raman microspectrometry (RMS), and attenuated total reflectance Fourier transform infrared spectroscopic (ATR-FTIR) imaging were applied in combination for the analysis of the same individual airborne particles for the first time. After examining individual particles of micrometer size by low-Z particle EPMA, consecutive examinations by RMS and ATR-FTIR imaging of the same individual particles were then performed. The relocation of the same particles on Al or Ag foils was successfully carried out among the three standalone instruments for several standard samples and an indoor airborne particle sample, resulting in the successful acquisition of quality spectral data from the three single-particle analytical techniques. The combined application of the three techniques to several different standard particles confirmed that those techniques provided consistent and complementary chemical composition information on the same individual particles. Further, it was clearly demonstrated that the three different types of spectral and imaging data from the same individual particles in an indoor aerosol sample provided richer information on physicochemical characteristics of the particle ensemble than that obtainable by the combined use of two single-particle analytical techniques.

Structural characterization of biomedical Co-Cr-Mo components produced by direct metal laser sintering.

PubMed

Barucca, G; Santecchia, E; Majni, G; Girardin, E; Bassoli, E; Denti, L; Gatto, A; Iuliano, L; Moskalewicz, T; Mengucci, P

2015-03-01

Direct metal laser sintering (DMLS) is a technique to manufacture complex functional mechanical parts from a computer-aided design (CAD) model. Usually, the mechanical components produced by this procedure show higher residual porosity and poorer mechanical properties than those obtained by conventional manufacturing techniques. In this work, a Co-Cr-Mo alloy produced by DMLS with a composition suitable for biomedical applications was submitted to hardness measurements and structural characterization. The alloy showed a hardness value remarkably higher than those commonly obtained for the same cast or wrought alloys. In order to clarify the origin of this unexpected result, the sample microstructure was investigated by X-ray diffraction (XRD), electron microscopy (SEM and TEM) and energy dispersive microanalysis (EDX). For the first time, a homogeneous microstructure comprised of an intricate network of thin ε (hcp)-lamellae distributed inside a γ (fcc) phase was observed. The ε-lamellae grown on the {111}γ planes limit the dislocation slip inside the γ (fcc) phase, causing the measured hardness increase. The results suggest possible innovative applications of the DMLS technique to the production of mechanical parts in the medical and dental fields. Copyright © 2014 Elsevier B.V. All rights reserved.

Imaging interactions of metal oxide nanoparticles with macrophage cells by ultra-high resolution scanning electron microscopy techniques.

PubMed

Plascencia-Villa, Germán; Starr, Clarise R; Armstrong, Linda S; Ponce, Arturo; José-Yacamán, Miguel

2012-11-01

Use of engineered metal oxide nanoparticles in a plethora of biological applications and custom products has warned about some possible dose-dependent cytotoxic effects. Macrophages are key components of the innate immune system used to study possible toxic effects and internalization of different nanoparticulate materials. In this work, ultra-high resolution field emission scanning electron microscopy (FE-SEM) was used to offer new insights into the dynamical processes of interaction of nanomaterials with macrophage cells dosed with different concentrations of metal oxide nanoparticles (CeO(2), TiO(2) and ZnO). The versatility of FE-SEM has allowed obtaining a detailed characterization of processes of adsorption and endocytosis of nanoparticles, by using advanced analytical and imaging techniques on complete unstained uncoated cells, including secondary electron imaging, high-sensitive backscattered electron imaging, X-ray microanalysis and stereoimaging. Low voltage BF/DF-STEM confirmed nanoparticle adsorption and internalization into endosomes of CeO(2) and TiO(2), whereas ZnO develop apoptosis after 24 h of interaction caused by dissolution and invasion of cell nucleus. Ultra-high resolution scanning electron microscopy techniques provided new insights into interactions of inorganic nanoparticles with macrophage cells with high spatial resolution.

Scanning electron microscopy study of new bone formation following small and large defects preserved with xenografts supplemented with pamidronate-A pilot study in Fox-Hound dogs at 4 and 8 weeks.

PubMed

Lozano-Carrascal, Naroa; Satorres-Nieto, Marta; Delgado-Ruiz, Rafael; Maté-Sánchez de Val, José Eduardo; Gehrke, Sergio Alexandre; Gargallo-Albiol, Jorge; Calvo-Guirado, José Luis

2017-01-01

The aim of the present study was to evaluate the feasibility of SEM and EDX microanalysis on evaluating the effect of porcine xenografts (MP3 ® ) supplemented with pamidronate during socket healing. Mandibular second premolars (P2) and first molars (M1) were extracted from six Beagle dogs. P2 were categorized as small defects (SD) and M1 as large defects (LD). Four random groups were created: SC (small control defects with MP3 ® ), ST (small test defects MP3 ® +pamidronate), LC (large control defects with MP3 ® ), and LT (large test defects MP3 ® +pamidronate). At four and eight weeks of healing the samples were evaluated fisically through scanning electron microscopy (SEM), and chemical element mapping was carried out by Energy dispersive X-ray spectroscopy (EDX). After four weeks of healing, SEM and EDX analysis revealed more mineralized bone in ST and LT groups compared with control groups (p<0.05). After eight weeks, Ca/P ratios were slightly higher for small defects (groups SC and ST); in SEM description, in both control and test groups, trabecular bone density was similar to the adjacent mineralized cortical bone. Within the limitations of this experimental study, SEM description and EDX elemental microanalysis have demonstrated to be useful techniques to assess bone remodelling of small and large defects. Both techniques show increased bone formation in test groups (MP3 ® modified with pamidronate) after four and eight weeks of healing. Copyright © 2016 Elsevier GmbH. All rights reserved.

Rare earth element concentrations in geological and synthetic samples using synchrotron X-ray fluorescence analysis

USGS Publications Warehouse

Chen, J.R.; Chao, E.C.T.; Back, J.M.; Minkin, J.A.; Rivers, M.L.; Sutton, S.R.; Cygan, G.L.; Grossman, J.N.; Reed, M.J.

1993-01-01

The concentrations of rare earth elements (REEs) in specific mineral grains from the Bayan Obo ore deposit and synthetic high-silica glass samples have been measured by synchrotron X-ray fluorescence (SXRF) analysis using excitation of the REE K lines between 33 and 63 keV. Because SXRF, a nondestructive analytical technique, has much lower minimum detection limits (MDLs) for REEs, it is an important device that extends the in situ analytical capability of electron probe microanalysis (EPMA). The distribution of trace amounts of REEs in common rock-forming minerals, as well as in REE minerals and minerals having minor quantities of REEs, can be analyzed with SXRF. Synchrotron radiation from a bending magnet and a wiggler source at the National Synchrotron Light Source, Brookhaven National Laboratory, was used to excite the REEs. MDLs of 6 ppm (La) to 26 ppm (Lu) for 3600 s in 60-??m-thick standard samples were obtained with a 25-??m diameter wiggler beam. The MDLs for the light REEs were a factor of 10-20 lower than the MDLs obtained with a bending magnet beam. The SXRF REE concentrations in mineral grains greater than 25 ??m compared favorably with measurements using EPMA. Because EPMA offered REE MDLs as low as several hundred ppm, the comparison was limited to the abundant light REEs (La, Ce, Pr, Nd). For trace values of medium and heavy REEs, the SXRF concentrations were in good agreement with measurements using instrumental neutron activation analysis (INAA), a bulk analysis technique. ?? 1993.

Ultrastructure and chemical composition of the proboscis hooks of Acanthocephalus lucii (Müller, 1776) (Acanthocephala: Palaeacanthocephala) using X-ray elemental analysis.

PubMed

Brázová, Tímea; Poddubnaya, Larisa G; Miss, Noemí Ramírez; Hanzelová, Vladimíra

2014-12-01

The ultrastructure and chemical composition of the proboscis hooks and surrounding tegument of Acanthocephalus lucii (Müller, 1776), a parasite of European perch, Perca fluviatilis Linnaeus, were examined using scanning (SEM) and transmission (TEM) electron microscopy and X-ray microanalysis (EDXA). The blade of middle hooks consists of three layers: an outer homogeneous layer, an inner heterogeneous layer and a central core. TEM observation revealed the presence of hollow tubes, which spaced the central core; fibrous inner hook layer surrounded by an electron-dense margin and the basal tegumental layer filled with electron-dense bodies and outer layer. We found for the first time that the so-called 'epidermal covering' surrounding of the exposed hook blade (outer hook layer) is a modified striped portion of the tegumental layer and there are no special contact sites between these two morphologically different structures, i.e. striped layer of the syncytial tegument and following proper outer hook layer, which is a homogeneous, moderately electron-dense layer of -0.3 μm in thickness. The hook root is embedded into subtegumental fibrous layer. X-ray microanalysis of both the surface and internal parts of A. lucii hooks demonstrated the presence of calcium, magnesium, phosphorus and sulphur. The highest concentration of sulphur was recorded at the tip of hooks, whereas the middle part of the hooks was most rich in calcium, phosphorus and magnesium. The proximal part of the hooks contained lower concentrations of sulphur, calcium and phosphorus. In the proboscis tegument, only two elements, calcium and silicon, were found. The differences observed in the chemical composition of the hook 'epidermal covering' and the proboscis tegument support our ultrastructural findings that the hook tegumental covering is a modified structure compared with that of the general proboscis tegument.

Physicochemical characterization of raw materials and co-products from the titanium dioxide industry.

PubMed

Gázquez, M J; Bolívar, J P; García-Tenorio, R; Vaca, F

2009-07-30

The present study was conducted to characterize several raw materials and co-products from the titanium dioxide industry in relation to their elemental composition (major, minor and trace elements), granulometry, mineralogy, microscopic morphology and physical composition. The main objective was to gain basic information for the future potential application of these co-products in fields such as agriculture, construction, civil engineering, etc. Microscopic studies were performed by applying scanning electron microscopy with X-ray microanalysis (SEM-XRMA) while the mineralogical compositions were analysed by means of the X-ray diffraction (XRD) technique. The concentrations of major elements such as Na, Al, Si, Ca, Ti, Fe, S and K were determined by X-ray fluorescence (XRF), while heavy metals and other trace elements were determined by ICP-MS. The physicochemical characterization of the raw materials used in the titanium dioxide industry, in addition to the characterization of the co-products generated, has enabled the evaluation of the degree of fractionation of different elements and compounds between the different co-products, as well as the control of the possible variations in the physicochemical composition of the raw materials throughout the time and the study of the influence of these variations in the characteristics of the obtained co-products. As a main conclusion of our study, it is possible to indicate that the levels of the pollutant elements associated to the co-products analysed were, in general, within safe limits and, therefore, they could potentially be used in composites as fertilizers or for building materials in road construction, etc. Nevertheless, for the specific application of each of these co-products in agriculture, construction and civil engineering, additional studies need to be performed to evaluate their appropriateness for the proposed application, together with specific studies on their health and environmental impact.

Evaluation of laboratory powder X-ray micro-diffraction for applications in the fields of cultural heritage and forensic science.

PubMed

Svarcová, Silvie; Kocí, Eva; Bezdicka, Petr; Hradil, David; Hradilová, Janka

2010-09-01

The uniqueness and limited amounts of forensic samples and samples from objects of cultural heritage together with the complexity of their composition requires the application of a wide range of micro-analytical methods, which are non-destructive to the samples, because these must be preserved for potential late revision. Laboratory powder X-ray micro-diffraction (micro-XRD) is a very effective non-destructive technique for direct phase analysis of samples smaller than 1 mm containing crystal constituents. It compliments optical and electron microscopy with elemental micro-analysis, especially in cases of complicated mixtures containing phases with similar chemical composition. However, modification of X-ray diffraction to the micro-scale together with its application for very heterogeneous real samples leads to deviations from the standard procedure. Knowledge of both the limits and the phenomena which can arise during the analysis is crucial for the meaningful and proper application of the method. We evaluated basic limits of micro-XRD equipped with a mono-capillary with an exit diameter of 0.1 mm, for example the size of irradiated area, appropriate grain size, and detection limits allowing identification of given phases. We tested the reliability and accuracy of quantitative phase analysis based on micro-XRD data in comparison with conventional XRD (reflection and transmission), carrying out experiments with two-phase model mixtures simulating historic colour layers. Furthermore, we demonstrate the wide use of micro-XRD for investigation of various types of micro-samples (contact traces, powder traps, colour layers) and we show how to enhance data quality by proper choice of experiment geometry and conditions.

High-resolution elemental mapping of human placental chorionic villi using synchrotron X-ray fluorescence spectroscopy

DOE PAGES

Punshon, Tracy; Chen, Si; Finney, Lydia; ...

2015-07-03

The placenta is the organ that mediates transport of nutrients and waste materials between mother and fetus. Synchrotron X-ray fluorescence (SXRF) microanalysis is a tool for imaging the distribution and quantity of elements in biological tissue, which can be used to study metal transport across biological membranes. Our aims were to pilot placental biopsy specimen preparation techniques that could be integrated into an ongoing epidemiology birth cohort study without harming rates of sample acquisition. We studied the effects of fixative (formalin or glutaraldehyde) and storage duration (30 days or immediate processing) on metal distribution and abundance and investigated a thaw-fixationmore » protocol for archived specimens stored at -80° C. We measured fixative elemental composition with and without a placental biopsy via inductively coupled plasma mass spectrometry (ICP-MS) to quantify fixative-induced elemental changes. Formalin-fixed specimens showed hemolysis of erythrocytes. The glutaraldehyde-paraformaldehyde solution in HEPES buffer (GTA-HEPES) had superior anatomical preservation, avoided hemolysis, and minimized elemental loss, although some cross-linking of exogenous Zn was evident. Elemental loss from tissue stored in fixative for 1 month showed variable losses (≈ 40 % with GTA-HEPES), suggesting storage duration be controlled for. Lastly, thawing of tissue held at -80 °C in a GTA-HEPES solution provided high-quality visual images and elemental images« less

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

PubMed

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.

Dopant-Site Determination in Y- and Sc-Doped (Ba0.5Sr0.5)(Co0.8Fe0.2)O3-δ by Atom Location by Channeling Enhanced Microanalysis and the Role of Dopant Site on Secondary Phase Formation.

PubMed

Meffert, Matthias; Störmer, Heike; Gerthsen, Dagmar

2016-02-01

(Ba0.5Sr0.5)(Co0.8Fe0.2)O3-δ (BSCF) is a promising material with mixed ionic and electronic conductivity which is considered for oxygen separation membranes. Selective improvement of material properties, e.g. oxygen diffusivity or suppression of secondary phase formation, can be achieved by B-site doping. This study is concerned with the formation of Co-oxide precipitates in undoped BSCF at typical homogenization temperatures of 1,000°C, which act as undesirable nucleation sites for other secondary phases in the application-relevant temperature range. Y-doping successfully suppresses Co-oxide formation, whereas only minor improvements are achieved by Sc-doping. To understand the reason for the different behavior of Y and Sc, the lattice sites of dopant cations in BSCF were experimentally determined in this work. Energy-dispersive X-ray spectroscopy in a transmission electron microscope was applied to locate dopant sites exploiting the atom location by channeling enhanced microanalysis technique. It is shown that Sc exclusively occupies B-cation sites, whereas Y is detected on A- and B-cation sites in Y-doped BSCF, although solely B-site doping was intended. A model is presented for the suppression of Co-oxide formation in Y-doped BSCF based on Y double-site occupancy.

Novel preparation of highly photocatalytically active copper chromite nanostructured material via a simple hydrothermal route

PubMed Central

Beshkar, Farshad; Zinatloo-Ajabshir, Sahar; Bagheri, Samira; Salavati-Niasari, Masoud

2017-01-01

Highly photocatalytically active copper chromite nanostructured material were prepared via a novel simple hydrothermal reaction between [Cu(en)2(H2O)2]Cl2 and [Cr(en)3]Cl3.3H2O at low temperature, without adding any pH regulator or external capping agent. The as-synthesized nanostructured copper chromite was analyzed by transmission electron microscopy (TEM), UV–vis diffuse reflectance spectroscopy, energy dispersive X-ray microanalysis (EDX), scanning electron microscopy (SEM), X-ray diffraction (XRD) and Fourier transform infrared (FT-IR) spectroscopy. Results of the morphological investigation of the as-synthesized products illustrate that the shape and size of the copper chromite depended on the surfactant sort, reaction duration and temperature. Moreover, the photocatalytic behavior of as-obtained copper chromite was evaluated by photodegradation of acid blue 92 (anionic dye) as water pollutant. PMID:28582420

Rapid and solvent-free solid-state synthesis and characterization of Zn3V2O8 nanostructures and their phenol red aqueous solution photodegradation

NASA Astrophysics Data System (ADS)

Mazloom, Fatemeh; Masjedi-Arani, Maryam; Salavati-Niasari, Masoud

2017-08-01

Zinc vanadate (Zn3V2O8) nanostructures have been successfully synthesized via simple, rapid and solvent-free solid-state method by using different complex precursors of Zn and NH4VO3 as novel starting materials. Effects of various zinc (II) Schiff base complex precursors and calcination temperatures were investigated to reach optimum condition. It was found that particle size and optical property of the as-prepared products could be greatly influenced via these parameters. The products were characterized by X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectra, energy dispersive X-ray microanalysis (EDX), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Photoluminescence and ultraviolet-visible (UV-Vis) spectroscopy. The photocatalytic activity of zinc vanadate nano and bulk structures were compared by degradation of phenol red aqueous solution.

Synthesis, spectroscopy and computational studies of some biologically important hydroxyhaloquinolines and their novel derivatives

NASA Astrophysics Data System (ADS)

Malecki, Grzegorz; Nycz, Jacek E.; Ryrych, Ewa; Ponikiewski, Lukasz; Nowak, Maria; Kusz, Joachim; Pikies, Jerzy

2010-04-01

A series crystalline compounds of methyl and phosphinyl derivatives of 2-methylquinolin-8-ol ( 1a) and related 5,7-dichloro-2-methylquinolin-8-ol ( 1b) were quantitatively prepared and characterized by microanalysis, IR, UV-vis and multinuclear NMR spectroscopy. Five of them have been characterized by single crystal X-ray diffraction method. The known compounds, 8-methoxy-2-methylquinoline ( 2a) and 8-methoxyquinoline ( 2d), were synthesised by a new route. NMR solution spectra at ambient temperature, showed readily diagnostic H-1 and C-13 signals from methyl groups. The geometries of the studied compounds were optimized in singlet states using the density functional theory (DFT) method with B3LYP functional. In general, the predicted bond lengths and angles are in a good agreement with the values based on the X-ray crystal structure data. Electronic spectra were calculated by TDDFT method.

Surface characterization of ZnO/ZnMn2O4 and Cu/Mn3O4 powders obtained by thermal degradation of heterobimetallic complexes

NASA Astrophysics Data System (ADS)

Barrault, Joël; Makhankova, Valeriya G.; Khavryuchenko, Oleksiy V.; Kokozay, Vladimir N.; Ayrault, Philippe

2012-03-01

From the selective transformation of the heterometallic (Zn-Mn or Cu-Mn) carboxylate complexes with 2,2'-bipyridyl by thermal degradation at relatively low (350 °C) temperature, it was possible to get either well defined spinel ZnMn2O4 over zinc oxide or well dispersed copper particles surrounded by a manganese oxide (Mn3O4) in a core-shell like structure. Morphology of the powder surface was examined by scanning electron microscopy with energy dispersive X-ray microanalysis (SEM/EDX). Surface composition was determined by X-ray photoelectron spectroscopy (XPS). Specific surface of the powders by nitrogen adsorption was found to be 33±0.2 and 9±0.06 m2 g-1 for Zn-Mn and Cu-Mn samples, respectively, which is comparable to those of commercial products.

Application of SEM and EDX in studying biomineralization in plant tissues.

PubMed

He, Honghua; Kirilak, Yaowanuj

2014-01-01

This chapter describes protocols using formalin-acetic acid-alcohol (FAA) to fix plant tissues for studying biomineralization by means of scanning electron microscopy (SEM) and qualitative energy-dispersive X-ray microanalysis (EDX). Specimen preparation protocols for SEM and EDX mainly include fixation, dehydration, critical point drying (CPD), mounting, and coating. Gold-coated specimens are used for SEM imaging, while gold- and carbon-coated specimens are prepared for qualitative X-ray microanalyses separately to obtain complementary information on the elemental compositions of biominerals. During the specimen preparation procedure for SEM, some biominerals may be dislodged or scattered, making it difficult to determine their accurate locations, and light microscopy is used to complement SEM studies. Specimen preparation protocols for light microscopy generally include fixation, dehydration, infiltration and embedding with resin, microtome sectioning, and staining. In addition, microwave processing methods are adopted here to speed up the specimen preparation process for both SEM and light microscopy.

Electron-excited energy dispersive x-ray spectrometry in the variable pressure scanning electron microscope (EDS/VPSEM): it's not microanalysis anymore!

NASA Astrophysics Data System (ADS)

Newbury, Dale E.; Ritchie, Nicholas W. M.

2015-10-01

X-ray spectra suffer significantly degraded spatial resolution when measured in the variable-pressure scanning electron microscope (VPSEM, chamber pressure 1 Pa to 2500 Pa) as compared to highvacuum SEM (operating pressure < 10 mPa). Depending on the gas path length, electrons that are scattered hundreds of micrometers outside the focused beam can contribute 90% or more of the measured spectrum. Monte Carlo electron trajectory simulation, available in NIST DTSA-II, models the gas scattering and simulates mixed composition targets, e.g., particle on substrate. The impact of gas scattering at the major (C > 0.1 mass fraction), minor (0.01 <= C <= 0.1), and trace (C < 0.01) constituent levels can be estimated. NIST DTSA-II for Java-platforms is available free at: http://www.cstl.nist.gov/div837/837.02/epq/dtsa2/index.html).

Electrochemical characterization of nano-sized Pd-based catalysts as cathode materials in direct methanol fuel cells.

PubMed

Choi, M; Han, C; Kim, I T; An, J C; Lee, J J; Lee, H K; Shim, J

2011-01-01

To improve the catalytic activity of palladium (Pd) as a cathode catalyst in direct methanol fuel cells (DMFCs), we prepared palladium-titanium oxide (Pd-TiO2) catalysts which the Pd and TiO2 nanoparticles were simultaneously impregnated on carbon. We selected Pd and TiO2 as catalytic materials because of their electrochemical stability in acid solution. The crystal structure and the loading amount of Pd and TiO2 on carbon were characterized by X-ray diffraction (XRD) and energy dispersive X-ray microanalysis (EDX). The electrochemical characterization of Pd-TiO2/C catalysts for the oxygen reduction reaction was carried out in half and single cell systems. The catalytic activities of the Pd-TiO2 catalysts were strongly influenced by the TiO2 content. In the single cell test, the Pd-TiO2 catalysts showed very comparable performance to the Pt catalyst.

IDM release behavior and surface characteristics of the novel Cu/IDM/LDPE nanocomposite for intrauterine device.

PubMed

Yang, Zhihong; Xie, Changsheng; Xiang, Hua; Feng, Jinqing; Xia, Xianping; Cai, Shuizhou

2009-03-01

Copper/indomethacin/low-density polyethylene (Cu/IDM/LDPE) nanocomposite was prepared as a novel material for intra-uterine device (IUD). IDM release profile of the nanocomposite was investigated by using spectrophotometer. The results show that IDM release rate of Cu/IDM/LDPE nanocomposite is higher in simulated uterine solution than that in methanol, confirming that the release process of IDM is dominated mainly by pore diffusion. The decrease in copper particle size and the increase in copper mass content all accelerate IDM release, indicating that IDM release rate can be adjusted by changing copper loading or copper particle size. The surface of the incubated nanocomposite was characterized by X-ray diffraction, scanning electron microscopy and energy dispersive X-ray microanalysis. A few deposits composed of P, Cl, Ca, Cu and O were observed on the nanocomposite surface, which may be related to the presence of IDM particles with large particle size.

Modification of carbon composites by nanoceramic compounds

NASA Astrophysics Data System (ADS)

Stoch, A.; Jastrzebski, W.; Długoń, E.; Stoch, G. J.; Błażewicz, S.; Adamczyk, A.; Tatarzyńska, K.

2005-06-01

Carbon-carbon composites (C/C) exhibit excellent high-temperature mechanical properties but their air oxidation limits their use at temperatures above 500 °C to inert atmosphere. Variety of coatings has been used to protect C/C composites from oxidation. In this work C/C composite substrates were covered with ceramic multilayer coats by electrophoretic deposition from ceramic sols such as silica sol, alumina sol and silica-lumina sol. Sol particles were of nano-sized dimensions. Deposited coats were annealed at 900-1500 °C. Oxidation tests at 600 °C reveal that the best protection of C/C composite against oxidation gives the multilayer coat formed by three or four electrophoretic depositions. The phase composition in the final annealed layers was analyzed by Infrared spectroscopy (FTIR) and by X-ray diffraction analysis (XRD). Morphology and chemical composition was observed using Scanning electron microscopy (SEM) with energy dispersive X-ray microanalysis (EDS).

Ted Hall and the science of biological microprobe X-ray analysis: a historical perspective of methodology and biological dividends.

PubMed

Gupta, B L

1991-06-01

This review surveys the emergence of electron probe X-ray microanalysis as a quantitative method for measuring the chemical elements in situ. The extension of the method to the biological sciences under the influence of Ted Hall is reviewed. Some classical experiments by Hall and his colleagues in Cambridge, UK, previously unpublished, are described; as are some of the earliest quantitative results from the cryo-sections obtained in Cambridge and elsewhere. The progress of the methodology is critically evaluated from the earliest starts to the present state of the art. Particular attention has been focused on the application of the method in providing fresh insights into the role of ions in cell and tissue physiology and pathology. A comprehensive list of references is included for a further pursuit of the topics by the interested reader.

The microstructural characterization of an in situ grown Si{sub 3}N{sub 4} whisker-reinforced BAS glass-ceramic matrix composite

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

Yu, Feng; Ortiz-Longo, C.R.; White, K.W.

The microstructure of barium aluminum silicate (BAS)/silicon nitride in situ whisker reinforced ceramic matrix composite was examined by X-ray diffraction, transmission electron microscopy, electron diffraction and energy-dispersive X-ray microanalysis. Although the authors can not conclusively exclude the presence of orthorhombic BAS, hexagonal BAS and both {alpha}-Si{sub 3}N{sub 4} and {beta}-Si{sub 3}N{sub 4} were identified in this material. The {beta}-Si{sub 3}N{sub 4} whiskers nucleate and grow in random directions in the nearly continuous matrix of metastable hexacelsian. The crystallization process of the glass phase can be taken almost to completion but a small proportion of residual glass phase is present atmore » the interface and grains-junction. Both whisker-like and equiaxed {beta}-Si{sub 3}N{sub 4} exist in this material.« less

A new approach for the recovery of precious metals from solution and from leachates derived from electronic scrap.

PubMed

Macaskie, L E; Creamer, N J; Essa, A M M; Brown, N L

2007-03-01

A new approach is described for the recovery of precious metals (PMs: Au, Pd and Ag) with >99% efficiency from aqueous solution utilising biogas produced during the aerobic growth of Klebsiella pneumoniae. Gold was recovered from electronic scrap leachate ( approximately 95%) by this method, with some selectivity against Cu. The recovered PM solids all contained metal and sulphur as determined by energy dispersive X-ray microanalysis (EDX). X-ray powder diffraction analysis (XRD) showed no crystalline metal sulphur compounds but a crystalline palladium amine was recorded. Silver was recovered as a sulphide (found by EDX), carbonate and oxide (found by XRD). EDX analysis of the Au-precipitate showed mainly gold and sulphur, with some metallic Au(0) detected by XRD. The gold compound was shock-sensitive; upon grinding it detonated to leave a sooty black deposit.

Energetics of a uranothorite (Th 1–xU xSiO 4) solid solution

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

Guo, Xiaofeng; Szenknect, Stephanie; Mesbah, Adel

High-temperature oxide melt solution calorimetric measurements were completed to determine the enthalpies of formation of the uranothorite, (USiO 4) x–(ThSiO 4) 1–x, solid solution. Phase-pure samples with x values of 0, 0.11, 0.21, 0.35, 0.71, and 0.84 were prepared, purified, and characterized by powder X-ray diffraction, electron probe microanalysis, thermogravimetric analysis and differential scanning calorimetry coupled with in situ mass spectrometry, and high-temperature oxide melt solution calorimetry. This work confirms the energetic metastability of coffinite, USiO 4, and U-rich intermediate silicate phases with respect to a mixture of binary oxides. Furthermore, variations in unit cell parameters and negative excess volumesmore » of mixing, coupled with strongly exothermic enthalpies of mixing in the solid solution, suggest short-range cation ordering that can stabilize intermediate compositions, especially near x = 0.5.« less

Energetics of a uranothorite (Th 1–xU xSiO 4) solid solution

DOE PAGES

Guo, Xiaofeng; Szenknect, Stephanie; Mesbah, Adel; ...

2016-10-11

High-temperature oxide melt solution calorimetric measurements were completed to determine the enthalpies of formation of the uranothorite, (USiO 4) x–(ThSiO 4) 1–x, solid solution. Phase-pure samples with x values of 0, 0.11, 0.21, 0.35, 0.71, and 0.84 were prepared, purified, and characterized by powder X-ray diffraction, electron probe microanalysis, thermogravimetric analysis and differential scanning calorimetry coupled with in situ mass spectrometry, and high-temperature oxide melt solution calorimetry. This work confirms the energetic metastability of coffinite, USiO 4, and U-rich intermediate silicate phases with respect to a mixture of binary oxides. Furthermore, variations in unit cell parameters and negative excess volumesmore » of mixing, coupled with strongly exothermic enthalpies of mixing in the solid solution, suggest short-range cation ordering that can stabilize intermediate compositions, especially near x = 0.5.« less

[Polyethylene abrasion: cause or consequence of an endoprosthesis loosening? Investigations of firm and loosened hip implants].

PubMed

Busse, B; Niecke, M; Püschel, K; Delling, G; Katzer, A; Hahn, M

2007-01-01

Periprosthetic tissue was analysed by the combination of different investigation techniques without destruction. The localisation and geometry of polyethylene abrasion particles were determined quantitatively to differentiate between abrasion due to function and abrasion due to implant loosening. Non-polyethylene particles from implant components which contaminate the tissue were micro-analytically measured. The results will help us to understand loosening mechanisms and thus lead to implant optimisations. A non-destructive particle analysis using highly sensitive proton-induced X-ray emission (PIXE) was developed to achieve a better histological allocation. Five autopsy cases with firmly fitting hip endoprosthesis (2 x Endo-Modell Mark III, 1 x St. Georg Mark II, LINK, Germany; 2 x Spongiosa Metal II, ESKA, Germany) were prepared as ground tissue specimens. Wear investigations were accomplished with a combined application of different microscopic techniques and microanalysis. The abrasion due to implant loosening was histologically evaluated on 293 loosened cup implants (St. Georg Mark II, LINK, Germany). Wear particles are heterogeneously distributed in the soft tissue. In cases of cemented prostheses, cement particles are dominating whereas metal particles could rarely be detected. The concentration of the alloy constituent cobalt (Co) is increased in the mineralised bone tissue. The measured co-depositions depend on the localisation and/or lifetime of an implant. Functional polyethylene (PE) abrasion needs to be differentiated from PE abrasion of another genesis (loosening, impingement) morphologically and by different tissue reactions. In the past a reduction of abrasion was targeted primarily by the optimisation of the bearing surfaces and tribology. The interpretation of our findings indicates that different mechanisms of origin in terms of tissue contamination with wear debris and the alloy should be included in the improvement of implants or implantation techniques.

Influence of Cobalt on the Adhesion Strength of Polycrystalline Diamond Coatings on WC-Co Hard Alloys

NASA Astrophysics Data System (ADS)

Linnik, S. A.; Gaidaichuk, A. V.; Okhotnikov, V. V.

2018-02-01

The influence of cobalt on the phase composition and adhesion strength of polycrystalline diamond coatings has been studied using scanning electron microscopy, Raman spectroscopy, and X-ray microanalysis. The coatings have been deposited on WC-Co hard alloy substrates in glow discharge plasma. It has been found that the catalytic amorphization of carbon only takes place during the direct synthesis of the diamond coating, when the cobalt vapor pressure over the substrate is high and the cobalt-related degradation of the synthesized diamond is absent.

[Mechanism of renal elimination of 2 elements of group IIIA of the periodic table : aluminum and indium].

PubMed

Galle, P

1981-01-05

Aluminium and indium, two elements of group IIIA of the periodic table, are concentrated by the kidney inside lysosomes of proximal tubule cell. In these lysosomes, aluminium and indium are precipitated as non-soluble phosphate salts and these precipitates are then expelled in the tubular lumen and eliminated with the urinary flow. These data have been visualized by analytical microscopy (ion microscopy and X ray microanalysis). Local acid phosphatases are assumed to permit the concentration of aluminium and indium salts inside the lysosomes.

Forensic microanalysis of Manhattan Project legacy radioactive wastes in St. Louis, MO.

PubMed

Kaltofen, Marco; Alvarez, Robert; Hixson, Lucas W

2018-06-01

Radioactive particulate matter (RPM) in St Louis, MO, area surface soils, house dusts and sediments was examined by scanning electron microscopy with energy dispersive X-ray analysis. Analyses found RPM containing 238 U and decay products (up to 46 wt%), and a distinct second form of RPM containing 230 Th and decay products (up to 15.6 wt%). The SEM-EDS analyses found similar RPM in Manhattan Project-era radioactive wastes and indoor dusts in surrounding homes. Copyright © 2018 Elsevier Ltd. All rights reserved.

Electron Microscope Studies of Cadmium Mercury Telluride

NASA Astrophysics Data System (ADS)

Lyster, Martin

Available from UMI in association with The British Library. Requires signed TDF. Epitaxial layers of Cd_{x }Hg_{(1-x)}Te grown on various substrates by liquid phase epitaxy and metallo-organic vapour phase epitaxy have been studied using transmission and scanning electron microscopy, in a variety of contrast modes. Wavelength-dispersive X-ray microanalysis has been used to study interfaces in epitaxial specimens, and the results are used to derive diffusion coefficients for a range of values of x in Cd_ {x}Hg_{(1-x)} Te. Extensive use has been made of back-scattered electron contrast in the SEM as a means of compositional mapping, and defect structures are imaged by this technique. The back-scattered electron contrast at interfaces has been studied in detail and is modelled using the Monte Carlo approach. The modelling is combined with calculations and practical measurements of the probe size in the SEM instrument used in the work, to arrive at a quantitative explanation of this contrast. The SEM and scintillator detector used allow a spatial resolution of better than 1000A, but it is shown that improvements in this are possible with present technology. Scanning infra-red microscopy (SIRM) and high -resolution transmission electron microscopy (HREM) have been applied to the study of CdTe. SIRM images reveal information about Te precipitation, including particle size and density. HREM images provide results concerning dislocation structures in CdTe. Selected-area diffraction contrast TEM results are presented which illustrate the microstructure of LPE and MOVPE material; and TEM foil preparation techniques are discussed, including the choice of ion species for milling cross-sectional specimens. In view of the results obtained, suggestions are made for future work in this field.

Effect of Cooling Rates on γ → α Transformation and Metastable States in Fe-Cu Alloys with Addition of Ni

NASA Astrophysics Data System (ADS)

Crozet, C.; Verdier, M.; Lay, S.; Antoni-Zdziobek, A.

2018-07-01

α/γ phase transformations occurring in Fe-10Cu-xNi alloys (0 ≤ x ≤ 15 in mass%) were studied using X-ray diffraction, scanning electron microscopy, electron back scattered diffraction, transmission electron microscopy and chemical analysis, combining X-ray microanalysis with energy dispersive spectrometry in the scanning electron microscope and electron microprobe analysis with wavelength dispersive spectrometry. The influence of cooling rate on the microstructure was investigated using ice-brine quenching and 2 °C/min slow cooling rate performed with dilatometry. Ni addition induces metastable transformations on cooling: massive and bainitic ferrite are formed depending on the alloy composition and cooling rate. Moreover, most of the Cu phase precipitates on cooling giving rise to a fine distribution of Cu particles in the ferrite grains. For both cooling conditions, the hardness increases with increasing Ni content and a higher hardness is obtained in the quenched alloy for each composition. The change in hardness is correlated to the effect of Ni solid solution, transformation structure and size of Cu particles.

Rediscovering Ducos du Hauron's Color Photography through a Review of His Three-Color Printing Processes and Synchrotron Microanalysis of His Prints.

PubMed

Cotte, Marine; Fabris, Tiphaine; Langlois, Juliette; Bellot-Gurlet, Ludovic; Ploye, Françoise; Coural, Natalie; Boust, Clotilde; Gandolfo, Jean-Paul; Galifot, Thomas; Susini, Jean

2018-06-18

Louis Ducos du Huron (1837-1920) dedicated his entire life to the elaboration of physical-chemical processes for color photography. This study aimed at highlighting his unique contribution to three-color printing through 1) an in-depth review of the many protocols he published and 2) the synchrotron-based IR and X-ray microanalysis of fragments sampled in three artworks. Ducos du Hauron's method relied on the preparation and assembly of three monochromes (red, blue, yellow). This study brings to light complex multistep recipes based on photochemistry (carbon print), organic, and inorganic chemistry. The various ingredients involved (e.g., pigments, dichromate gelatin, collodion, resin) were identified and localized through their spectroscopic signature, confirming the relevance of synchrotron spectromicroscopy for the characterization of historical photographs. The impressive correlation between texts and chemical analyses calls for a wider application to the history of photography. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Correlated Microanalysis of Cometary Organic Grains Returned by Stardust

NASA Technical Reports Server (NTRS)

DeGregorio, B. T.; Stroud, R. M.; Nittler, L. R.; Cody, G. D,; Kilcoyne, A. L. D.

2011-01-01

Preliminary examination (PE) of samples returned from Comet 81P/Wild 2 by the NASA Stardust mission revealed a wide variety of carbonaceous samples [e.g. 1]. Carbonaceous matter is present as inclusions, rinds, and films in polyminerallic terminal particles [2-4], as carbon-rich particles along track walls [2, 5, 6], and as organic matter in aerogel around tracks [7, 8]. The organic chemistry of these samples ranges from purely aliphatic hydrocarbons to highly-aromatic material, often modified by various organic functional groups [2, 4, 5, 9-11]. Difficulty arises when interpreting the genesis of these carbonaceous samples, since contaminants could be introduced from the spacecraft [12], aerogel [1, 8], or during sample preparation. In addition, hypervelocity capture into aerogel may have heated cometary material in excess of 1000 C, which could have significantly altered the structure and chemistry of carbonaceous matter. Fortunately, much of this contamination or alteration can be identified through correlated microanalysis with transmission electron microscopy (TEM), scanning-transmission X-ray microscopy (STXM), and nanoscale secondary ion mass spectroscopy (SIMS).

A new basaltic glass microanalytical reference material for multiple techniques

USGS Publications Warehouse

Wilson, Steve; Koenig, Alan; Lowers, Heather

2012-01-01

The U.S. Geological Survey (USGS) has been producing reference materials since the 1950s. Over 50 materials have been developed to cover bulk rock, sediment, and soils for the geological community. These materials are used globally in geochemistry, environmental, and analytical laboratories that perform bulk chemistry and/or microanalysis for instrument calibration and quality assurance testing. To answer the growing demand for higher spatial resolution and sensitivity, there is a need to create a new generation of microanalytical reference materials suitable for a variety of techniques, such as scanning electron microscopy/X-ray spectrometry (SEM/EDS), electron probe microanalysis (EPMA), laser ablation inductively coupled mass spectrometry (LA-ICP-MS), and secondary ion mass spectrometry (SIMS). As such, the microanalytical reference material (MRM) needs to be stable under the beam, be homogeneous at scales of better than 10–25 micrometers for the major to ultra-trace element level, and contain all of the analytes (elements or isotopes) of interest. Previous development of basaltic glasses intended for LA-ICP-MS has resulted in a synthetic basaltic matrix series of glasses (USGS GS-series) and a natural basalt series of glasses (BCR-1G, BHVO-2G, and NKT-1G). These materials have been useful for the LA-ICP-MS community but were not originally intended for use by the electron or ion beam community. A material developed from start to finish with intended use in multiple microanalytical instruments would be useful for inter-laboratory and inter-instrument platform comparisons. This article summarizes the experiments undertaken to produce a basalt glass reference material suitable for distribution as a multiple-technique round robin material. The goal of the analytical work presented here is to demonstrate that the elemental homogeneity of the new glass is acceptable for its use as a reference material. Because the round robin exercise is still underway, only nominal compositional ranges for each element are given in the article.

Liquid phase electroepitaxial bulk growth of binary and ternary alloy semiconductors under external magnetic field

NASA Astrophysics Data System (ADS)

Sheibani, Hamdi

2002-01-01

Liquid Phase Electroepitaxy (LPEE) and is a relatively new, promising technique for producing high quality, thick compound semiconductors and their alloys. The main objectives are to reduce the adverse effect of natural convection and to determine the optimum growth conditions for reproducible desired crystals for the optoelectronic and electronic device industry. Among the available techniques for suppressing the adverse effect of natural convection, the application of an external magnetic field seems the most feasible one. The research work in this dissertation consists of two parts. The first part is focused on the design and development of a state of the art LPEE facility with a novel crucible design, that can produce bulk crystals of quality higher than those achieved by the existing LPEE system. A growth procedure was developed to take advantage of this novel crucible design. The research of the growth of InGaAs single crystals presented in this thesis will be a basis for the future LPEE growth of other important material and is an ideal vehicle for the development of a ternary crystal growth process. The second part of the research program is the experimental study of the LPEE growth process of high quality bulk single crystals of binary/ternary semiconductors under applied magnetic field. The compositional uniformity of grown crystals was measured by Electron Probe Micro-analysis (EPMA) and X-ray microanalysis. The state-of-the-art LPEE system developed at University of Victoria, because of its novel design features, has achieved a growth rate of about 4.5 mm/day (with the application of an external fixed magnetic field of 4.5 KGauss and 3 A/cm2 electric current density), and a growth rate of about 11 mm/day (with 4.5 KGauss magnetic field and 7 A/cm2 electric current density). This achievement is simply a breakthrough in LPEE, making this growth technique absolutely a bulk growth technique and putting it in competition with other bulk growth techniques. The growth rates achieved can even be higher for higher electric current and magnetic field intensities. (Abstract shortened by UMI.)

Cytology of pollutant metals in marine invertebrates: A review of microanalytical applications

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

Nott, J.A.

1991-03-01

x-ray microanalysis (XRMA) is customized for investigations of the metabolic and detoxification strategies of heavy metals taken by marine organisms from polluted environments. Sites of uptake, intracellular accumulation, transport and excretion are visualized, analysed and quantified. Cryopreparation techniques are required to prevent the translocation or loss from specimens of soluble metal species. In marine invertebrates, metals are detoxified by systems of chemical binding and intracellular compartmentalization. XRMA investigations have concentrated on marine molluscs and crustaceans and even within these restricted groups there are marked inter-species differences in the biochemical and cytological processes which reduce metal bioavailability. Some detoxification systems alsomore » protect the carnivores which ingest the metal-laden tissues of the prey. This results in the bioreduction of metals along a food chain. These processes are investigated by XRMA which can be tuned to observe the complex interactions which operate at all levels within and between the biota and polluted environments. 90 refs.« less

Integrated Experimental and Modelling Research for Non-Ferrous Smelting and Recycling Systems

NASA Astrophysics Data System (ADS)

Jak, Evgueni; Hidayat, Taufiq; Shishin, Denis; Mehrjardi, Ata Fallah; Chen, Jiang; Decterov, Sergei; Hayes, Peter

The chemistries of industrial pyrometallurgical non-ferrous smelting and recycling processes are becoming increasingly complex. Optimisation of process conditions, charge composition, temperature, oxygen partial pressure, and partitioning of minor elements between phases and different process streams require accurate description of phase equilibria and thermodynamics which are the focus of the present research. The experiments involve high temperature equilibration in controlled gas atmospheres, rapid quenching and direct measurement of equilibrium phase compositions with quantitative microanalytical techniques including electron probe X-ray microanalysis and Laser Ablation ICP-MS. The thermodynamic modelling is undertaken using computer package FactSage with the quasi-chemical model for the liquid slag phase and other advanced models. Experimental and modelling studies are combined into an integrated research program focused on the major elements Cu-Pb-Fe-O-Si-S system, slagging Al, Ca, Mg and other minor elements. The ongoing development of the research methodologies has resulted in significant advances in research capabilities. Examples of applications are given.

Viscosity Measurements of SiO2-"FeO"-MgO System in Equilibrium with Metallic Fe

NASA Astrophysics Data System (ADS)

Chen, Mao; Raghunath, Sreekanth; Zhao, Baojun

2014-01-01

The present study delivers the measurements of viscosities in the SiO2-"FeO"-MgO system in equilibrium with metallic Fe. The rotational spindle technique was used for the measurements at the temperature range of 1523 K to 1773 K (1250 °C to 1500 °C). Molybdenum crucibles and spindles were employed in all measurements. The viscosity measurements were carried out at 31 to 47 mol pct SiO2 and up to 18.8 mol pct MgO. Analysis of the quenched sample by Electron probe X-ray microanalysis after the viscosity measurement enables the composition and microstructure of the slag to be directly linked with the viscosity. The replacement of "FeO" by MgO was found to increase viscosity and activation energy of the SiO2-"FeO"-MgO slags. The modified Quasi-chemical Viscosity Model was further optimized in this system based on the current viscosity measurements.

The osteoplastic effectiveness of the implants made of mesh titanium nickelide constructs

PubMed Central

Irianov, Iurii Mikhailovich; Diuriagina, Olga Vladimirovna; Karaseva, Tatiana Iurevna; Karasev, Evgenii Anatolevich

2014-01-01

The purpose of the work was to study the features of reparative osteogenesis for filling the defect of tubular bone under implantation of mesh titanium nickelide constructs. Tibial fenestrated defect was modeled experimentally in 30 Wistar pubertal rats, followed by implant intramedullary insertion. The techniques of radiography, scanning electron microscopy and X-ray electron probe microanalysis were used. The mesh implant of titanium nickelide has been established to possess biocompatibility, osteoconductive and osteoinductive properties, the zone of osteogenesis and angiogenesis is created around it, bone cover is formed. Osteointegration of the implant occurs early, by 7 days after surgery, and by 30 days after surgery organotypical re-modelling of the regenerated bone takes place, as well as the defect is filled with lamellar bone tissue by the type of bone wound primary adhesion. By 30 days after surgery mineral content of the regenerated bone tissue approximates to the composition of intact cortex mineral phase. PMID:24579962

Experimental Investigation of Gas/Slag/Matte/Spinel Equilibria in the Cu-Fe-O-S-Si System at 1473 K (1200 °C) and P(SO2) = 0.25 atm

NASA Astrophysics Data System (ADS)

Hidayat, Taufiq; Fallah-Mehrjardi, Ata; Hayes, Peter C.; Jak, Evgueni

2018-04-01

New experimental data were obtained on the gas/slag/matte/spinel equilibria in the Cu-Fe-O-S-Si system at 1473 K (1200 °C) and P(SO2) = 0.25 atm covering Cu concentrations in matte between 42 and 78 wt pct Cu. Accurate measurements were obtained using high-temperature equilibration and the rapid quenching technique, followed by electron-probe X-ray microanalysis of equilibrium phase compositions. The use of spinel substrates made to support the samples ensures equilibrium with this primary phase solid, eliminates crucible contamination, and facilitates direct gas-condensed phase equilibrium and high quenching rates. Particular attention was given to the confirmation of the achievement of equilibrium. The results quantify the relationship between Cu in matte and oxygen partial pressure, sulfur in matte, oxygen in matte, Fe/SiO2 at slag liquidus, sulfur in slag, and dissolved copper in slag.

Characterization of Impact Damage in Ultra-High Performance Concrete Using Spatially Correlated Nanoindentation/SEM/EDX

NASA Astrophysics Data System (ADS)

Moser, R. D.; Allison, P. G.; Chandler, M. Q.

2013-12-01

Little work has been done to study the fundamental material behaviors and failure mechanisms of cement-based materials including ordinary Portland cement concrete and ultra-high performance concretes (UHPCs) under high strain impact and penetration loads at lower length scales. These high strain rate loadings have many possible effects on UHPCs at the microscale and nanoscale, including alterations in the hydration state and bonding present in phases such as calcium silicate hydrate, in addition to fracture and debonding. In this work, the possible chemical and physical changes in UHPCs subjected to high strain rate impact and penetration loads were investigated using a novel technique wherein nanoindentation measurements were spatially correlated with images using scanning electron microscopy and chemical composition using energy dispersive x-ray microanalysis. Results indicate that impact degrades both the elastic modulus and indentation hardness of UHPCs, and in particular hydrated phases, with damage likely occurring due to microfracturing and debonding.

Glass Formation, Phase Equilibria, and Thermodynamic Assessment of the Al-Ce-Co System Assisted by First-Principles Energy Calculations

NASA Astrophysics Data System (ADS)

Gao, Michael C.; Ünlü, Necip; Mihalkovic, Marek; Widom, Michael; Shiflet, G. J.

2007-10-01

This study investigates glass formation, phase equilibria, and thermodynamic descriptions of the Al-rich Al-Ce-Co ternary system using a novel approach that combines critical experiments, CALPHAD modeling, and first-principles (FP) calculations. The glass formation range (GFR) and a partial 500 °C isotherm are determined using a range of experimental techniques including melt spinning, transmission electron microscopy (TEM), electron probe microanalysis (EPMA), X-ray diffraction, and differential thermal analysis (DTA). Three stable ternary phases are confirmed, namely, Al8CeCo2, Al4CeCo, and AlCeCo, while a metastable phase, Al5CeCo2, was discovered. The equilibrium and metastable phases identified by the present and earlier reported experiments, together with many hypothetical ternary compounds, are further studied by FP calculations. Based on new experimental data and FP calculations, the thermodynamics of the Al-rich Al-Co-Ce system is optimized using the CALPHAD method. Application to glass formation is discussed in light of present studies.

Identification of phases in the interaction layer between U-Mo-Zr/Al and U-Mo-Zr/Al-Si

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

Varela, C.L. Komar; Arico, S.F.; Mirandou, M.

Out-of-pile diffusion experiments were performed between U-7wt.% Mo-1wt.% Zr and Al or Al A356 (7,1wt.% Si) at 550 deg. C. In this work morphological characterization and phase identification on both interaction layer are presented. They were carried out by the use of different techniques: optical and scanning electron microscopy, X-Ray diffraction and WDS microanalysis. In the interaction layer U-7wt.% Mo-1wt.% Zr/Al, the phases UAl{sub 3}, UAl{sub 4}, Al{sub 20}Mo{sub 2}U and Al{sub 43}Mo{sub 4}U{sub 6} were identified. In the interaction layer U-7wt.% Mo-1wt.% Zr/Al A356, the phases U(Al, Si) with 25at.% Si and Si{sub 5}U{sub 3} were identified. This lastmore » phase, with a higher Si concentration, was identified with XRD Synchrotron radiation performed at the National Synchrotron Light Laboratory (LNLS), Campinas, Brasil. (author)« less

X-ray microanalytical studies of mineral elements in the tripartite symbiosis between lima bean, N2-fixing bacteria and mycorrhizal fungi.

PubMed

Rodak, Bruna Wurr; Freitas, Douglas Siqueira; Bamberg, Soraya Marx; Carneiro, Marco Aurélio Carbone; Guilherme, Luiz Roberto Guimarães

2017-01-01

The symbiosis between legumes, arbuscular mycorrhizal (AM) fungi, and N 2 -fixing bacteria (NFB) provides mutual nutritional gains. However, assessing the nutritional status of the microorganisms is a difficult task. A methodology that could assess this status, in situ, could assist managing these organisms in agriculture. This study used X-ray microanalyses to quantify and locate mineral elements in structures formed in a tripartite symbiosis. Lima bean (Phaseolus lunatus L. Walp) was cultivated in pots under greenhouse conditions, to which we have added AM fungal isolates (Glomus macrocarpum and Acaulospora colombiana) and NFB (Bradyrhizobium japonicum) inocula. Uninoculated control plants were also included. Symbionts were evaluated at the onset of flowering. Quantification of the mineral elements in the symbiotic components was performed using energy dispersive X-ray spectroscopy (EDX) and a scanning electron microscopy (SEM) was used to identify structures. EDX analysis detected 13 elements with the most abundant being N, Ca, and Se, occurring in all tissues, Fe in roots, Ni and Al in epidermis and P and Mo in nodules. Elemental quantification in fungal structures was not possible. The distribution of elements was related to their symbiotic function. X-ray microanalysis can be efficiently applied for nutritional diagnosis in tripartite symbiosis. Copyright © 2016 Elsevier B.V. All rights reserved.

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

NASA Astrophysics Data System (ADS)

Chen, Zewu

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

Flash X-ray with image enhancement applied to combustion events

NASA Astrophysics Data System (ADS)

White, K. J.; McCoy, D. G.

1983-10-01

Flow visualization of interior ballistic processes by use of X-rays has placed more stringent requirements on flash X-ray techniques. The problem of improving radiographic contrast of propellants in X-ray transparent chambers was studied by devising techniques for evaluating, measuring and reducing the effects of scattering from both the test object and structures in the test area. X-ray film and processing is reviewed and techniques for evaluating and calibrating these are outlined. Finally, after X-ray techniques were optimized, the application of image enhancement processing which can improve image quality is described. This technique was applied to X-ray studies of the combustion of very high burning rate (VHBR) propellants and stick propellant charges.

A System Approach to Navy Medical Education and Training. Appendix 13. Dental Technician.

DTIC Science & Technology

1974-08-31

BOOKLET 26 ISELECT ALTERNATIVE TECHNIQUES IN SETTING X-PAY ONIT 27 IWRITE EXoOSURE TECHNIQUE CHAPT FOR X-RAY 28 ITAKE X-RAYS WITH A CEPHALID TUBE TILT...29 ITAKE X-PAYS WITH A CAUDAL TUBE TILT 30 ITAKE X-RAYS USING SCREEN TECHNIQUE 31 ITAKE X-RAYS USING FIXED GRID TECHNIQUE 32 ITAKE X-RAYS USING...MOULDS 31 IFABRICATE PLASTIC HEAD CAPS 32 IFABRICATE INTERNAL FACIAL PROSTHESIS 33 100 PROSTHETIC RECONSTRUCTION OF THE NOSE 34 IFABRICATE CUSTOM OCULAR

Analysis of Roman age wall paintings found in Pordenone, Trieste and Montegrotto.

PubMed

Mazzocchin, G A; Agnoli, F; Salvadori, M

2004-10-20

The aim of the present work is the study of many fragments of wall painting from archaeological excavations in three different Roman age sites dating back to the I Century before Common Era: Pordenone (località Torre); Trieste (Crosada) and Padova (Montegrotto). The techniques used were optical microscopy, scanning electron microscopy (SEM), equipped with a EDS microanalysis detector, X-rays powder diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), Fourier transform Raman spectroscopy (FT-Raman) and electron paramagnetic resonance (EPR) spectroscopy. The identified pigments were: cinnabar, hematite, celadonite, glauconite, cuprorivaite (Egyptian blue), yellow and red ochre, calcite, limonite, coal black. In general, the mortar preparation did not correspond to the complex procedure suggested by Vitruvius (De Architectura), but generally showed a porous layer, with crushed grains under the pigment layer. In some cases, two superimposed pigment layers were found: yellow superimposed on both red and pink, black on pink, green on black. The slight differences we found in the use of the pigments in the three studied sites might show that the same technology, culture and taste spread all over the Roman Empire in North Eastern Italy (X(a) Regio Venetia et Histria).

Blue light-dependent changes in loosely bound calcium in Arabidopsis mesophyll cells: an X-ray microanalysis study

PubMed Central

Łabuz, Justyna; Samardakiewicz, Sławomir; Hermanowicz, Paweł; Wyroba, Elżbieta; Pilarska, Maria; Gabryś, Halina

2016-01-01

Calcium is involved in the signal transduction pathway from phototropins, the blue light photoreceptor kinases which mediate chloroplast movements. The chloroplast accumulation response in low light is controlled by both phot1 and phot2, while only phot2 is involved in avoidance movement induced by strong light. Phototropins elevate cytosolic Ca2+ after activation by blue light. In higher plants, both types of chloroplast responses depend on Ca2+, and internal calcium stores seem to be crucial for these processes. Yet, the calcium signatures generated after the perception of blue light by phototropins are not well understood. To characterize the localization of calcium in Arabidopsis mesophyll cells, loosely bound (exchangeable) Ca2+ was precipitated with potassium pyroantimonate and analyzed by transmission electron microscopy followed by energy-dispersive X-ray microanalysis. In dark-adapted wild-type Arabidopsis leaves, calcium precipitates were observed at the cell wall, where they formed spherical structures. After strong blue light irradiation, calcium at the apoplast prevailed, and bigger, multilayer precipitates were found. Spherical calcium precipitates were also detected at the tonoplast. After red light treatment as a control, the precipitates at the cell wall were smaller and less numerous. In the phot2 and phot1phot2 mutants, calcium patterns were different from those of wild-type plants. In both mutants, no elevation of calcium after blue light treatment was observed at the cell periphery (including the cell wall and a fragment of cytoplasm). This result confirms the involvement of phototropin2 in the regulation of Ca2+ homeostasis in mesophyll cells. PMID:26957564

X-Ray Microanalysis of Human Cementum

NASA Astrophysics Data System (ADS)

Alvarez-Pérez, Marco Antonio; Alvarez-Fregoso, Octavio; Ortiz-López, Jaime; Arzate, Higinio

2005-08-01

An energy dispersive x-ray microanalysis study was performed throughout the total length of cementum on five impacted human teeth. Mineral content of calcium, phosphorous, and magnesium were determined with an electron probe from the cemento-enamel junction to the root apex on the external surface of the cementum. The concentration profiles for calcium, phosphorous, and magnesium were compared by using Ca/P and Mg/Ca atomic percent ratio. Our findings demonstrated that the Ca/P ratio at the cemento-enamel junction showed the highest values (1.8 2.2). However, the area corresponding to the acellular extrinsic fiber cementum (AEFC) usually located on the coronal one-third of the root surface showed a Ca/P media value of 1.65. Nevertheless, on the area representing the fulcrum of the root there is an abrupt change in the Ca/P ratio, which decreases to 1.3. Our results revealed that Mg2+ distribution throughout the length of human cementum reached its maximum Mg/Ca ratio value of 1.3 1.4 at.% around the fulcrum of the root and an average value of 0.03%. A remarkable finding was that the Mg/Ca ratio pattern distribution showed that in the region where the Ca/P ratio showed a decreasing tendency, the Mg/Ca ratio reached its maximum value, showing a negative correlation. In conclusion, this study has established that clear compositional differences exist between AEFC and cellular mixed stratified cementum varieties and adds new knowledge about Mg2+ distribution and suggests its provocative role regulating human cementum metabolism.

A multi-analytical study of the fifteenth century mural paintings of the Batalha Monastery (Portugal) in view of their conservation

NASA Astrophysics Data System (ADS)

Valadas, S.; Candeias, A.; Dias, C.; Schiavon, N.; Cotovio, M.; Pestana, J.; Gil, M.; Mirão, J.

2013-12-01

The systematic characterization of the painting's palette and technique applied on the execution of the mural paintings of the Batalha Monastery (Batalha, Leiria, Portugal) is presented. These are the oldest mural paintings known in Portugal (apart from Roman frescoes) and represent the beginning of an artistic Portuguese tradition that continues until the nineteenth century. The aim of the study was to identify for the first time by adopting a multi-analytical physico-chemical approach of the pigments, binder, and alteration products (white veils, crusts, and pigment alteration) of these unique works of arts in order not only to better understand the painting technique, but also to support a conservation-restoration intervention that took place from April to August 2010. Micro-sampling of paint layers was performed on representative areas of the paintings. The characterization of the pigments and binders was carried out by microscopy and microanalysis of cross sections using optical microscopy, scanning electron microscopy coupled with energy dispersive X-ray spectrometry (SEM-EDS), micro-FTIR, and micro X-ray diffraction. The combined analysis of the paintings allowed the identification of the painting's palette: Vermillion (HgS) and red ochre for the reds, yellow ochres for the yellows, green earths and malachite for the greens, azurite for the blues, and carbon for the blacks. The use of the pigment is dependent of the motive painted while the most expensive materials were used in the most important iconographic motives. Alteration of malachite was identified in darkened layers in green areas of the paintings. White veil areas on the surface of the paintings were identified as calcite from precipitation/dissolution processes due to water run-off on the sacristy dome ceiling and walls.

Recent results of synchrotron radiation induced total reflection X-ray fluorescence analysis at HASYLAB, beamline L

NASA Astrophysics Data System (ADS)

Streli, C.; Pepponi, G.; Wobrauschek, P.; Jokubonis, C.; Falkenberg, G.; Záray, G.; Broekaert, J.; Fittschen, U.; Peschel, B.

2006-11-01

At the Hamburger Synchrotronstrahlungslabor (HASYLAB), Beamline L, a vacuum chamber for synchrotron radiation-induced total reflection X-ray fluorescence analysis, is now available which can easily be installed using the adjustment components for microanalysis present at this beamline. The detector is now in the final version of a Vortex silicon drift detector with 50-mm 2 active area from Radiant Detector Technologies. With the Ni/C multilayer monochromator set to 17 keV extrapolated detection limits of 8 fg were obtained using the 50-mm 2 silicon drift detector with 1000 s live time on a sample containing 100 pg of Ni. Various applications are presented, especially of samples which are available in very small amounts: As synchrotron radiation-induced total reflection X-ray fluorescence analysis is much more sensitive than tube-excited total reflection X-ray fluorescence analysis, the sampling time of aerosol samples can be diminished, resulting in a more precise time resolution of atmospheric events. Aerosols, directly sampled on Si reflectors in an impactor were investigated. A further application was the determination of contamination elements in a slurry of high-purity Al 2O 3. No digestion is required; the sample is pipetted and dried before analysis. A comparison with laboratory total reflection X-ray fluorescence analysis showed the higher sensitivity of synchrotron radiation-induced total reflection X-ray fluorescence analysis, more contamination elements could be detected. Using the Si-111 crystal monochromator also available at beamline L, XANES measurements to determine the chemical state were performed. This is only possible with lower sensitivity as the flux transmitted by the crystal monochromator is about a factor of 100 lower than that transmitted by the multilayer monochromator. Preliminary results of X-ray absorption near-edge structure measurements for As in xylem sap from cucumber plants fed with As(III) and As(V) are reported. Detection limits of 170 ng/l of As in xylem sap were achieved.

Micro-chemical and metallurgical study of Samnite bronze belts from ancient Abruzzo (central Italy, VIII-IV BC)

NASA Astrophysics Data System (ADS)

Riccucci, Cristina; Ingo, Gabriel Maria; Faustoferri, Amalia; Pierigè, Maria Isabella; Parisi, Erica Isabella; Di Carlo, Gabriella; De Caro, Tilde; Faraldi, Federica

2013-12-01

The Samnite bronze belts and the chest disk cuirasses (VIII-IV BC) are the distinctive defensive weapons of the Samnite warriors having likely also a symbolic relevance. These artefacts were mainly found during the archaeological excavations of warriors' graves from ancient Abruzzo (central Italy). Their chemical composition, metallurgical features and corrosion products formed during the long-term burial have been studied by means of the combined use of analytical techniques such as optical microscopy (OM), scanning electron microscopy coupled with energy-dispersive X-ray micro-analysis (SEM-EDS), X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD). The micro-chemical and structural results show that the bronze belts have often been produced by using unusual high-tin bronze alloys achieving a silver-like appearance and by performing tailored cycles of thermal treatments under reducing conditions and hot mechanical working aimed to shape the high-tin alloys in the form of a thin bronze sheet. Furthermore, the investigation has shown that the main alloying elements have been transformed during the burial into mineral species giving rise to the formation of stratified structures constituted by different mineral phases such as tin oxides, cuprous oxide (Cu2O) and copper carbonates (azurite (Cu3(CO3)2(OH)2 and malachite (CuCO3Cu(OH)2)) as well as dangerous chlorine-based compounds such as nantokite (CuCl) and atacamite (Cu2(OH)3Cl) polymorphs. This information evidences the strict interaction of the alloying elements with the soil components as well as the occurrence of the copper cyclic corrosion as a post-burial degradation phenomenon. The present study confirms that the combined micro-chemical and micro-structural investigation techniques such as SEM-EDS, XPS, XRD and OM can be successfully used to investigate the technological production processes of the ancient artefacts and to achieve the detailed micro-chemical and structural description of the corrosion products useful for the identification of degradation agents and mechanisms and, thereafter, to propose a reliable tailored strategy for the conservation.

Microanalysis of extended-test xenon hollow cathodes

NASA Technical Reports Server (NTRS)

Verhey, Timothy R.; Patterson, Michael J.

1991-01-01

Four hollow cathode electron sources were analyzed via boroscopy, scanning electron microscopy, energy dispersive x ray analysis, and x ray diffraction analysis. These techniques were used to develop a preliminary understanding of the chemistry of the devices that arise from contamination due to inadequate feed-system integrity and improper insert activation. Two hollow cathodes were operated in an ion thruster simulator at an emission current of 23.0 A for approximately 500 hrs. The two tests differed in propellant-feed systems, discharge power supplies, and activation procedures. Tungsten deposition and barium tungstate formation on the internal cathode surfaces occurred during the first test, which were believed to result from oxygen contamination of the propellant feed-system. Consequently, the test facility was upgraded to reduce contamination, and the test was repeated. The second hollow cathode was found to have experienced significantly less tungsten deposition. A second pair of cathodes examined were the discharge and the neutralizer hollow cathodes used in a life-test of a 30-cm ring-cusp ion thruster at a 5.5 kW power level. The cathodes' test history was documented and the post-test microanalyses are described. The most significant change resulting from the life-test was substantial tungsten deposition on the internal cathode surfaces, as well as removal of material from the insert surface. In addition, barium tungstate and molybdate were found on insert surfaces. As a result of the cathode examinations, procedures and approaches were proposed for improved discharge ignition and cathode longevity.

Composition and microstructure of maiolica from the museum of ceramics in Ascoli Piceno (Italy): evidences by electron microscopy and microanalysis

NASA Astrophysics Data System (ADS)

Gulmini, M.; Scognamiglio, F.; Roselli, G.; Vaggelli, G.

2015-09-01

The present work focuses on majolica objects from the collection of the museum of ceramic in Ascoli Piceno (Italy). The scientific investigation was performed on fragments detached from seven maiolicas attributed to the Castelli production (Abruzzi region) and one majolica from the Ascoli Piceno production (Marche region). The Castelli artifacts (late sixteenth-early eighteenth century) belong to the decorated style known as " compendiario." The piece from Ascoli Piceno recalls the decoration style of the other considered objects and is attributable to the "Paci" manufacture (first half of the nineteenth century). The selected objects were investigated by fiber optics reflectance spectroscopy, micro-X-ray fluorescence spectroscopy and scanning electron microscopy coupled with electron-dispersive X-ray spectrometry. The ceramic bodies of all objects are calcareous, whereas the glazes are lead-alkali type opacified by tin dioxide. Blue and purplish-red decorations were obtained by cobalt and manganese compounds dissolved in the glaze, respectively. Yellow and orange decorations were obtained by particles of lead antimonate and hematite. Finally, black decorations were obtained using compounds rich in manganese and iron. The study contributes to knowledge on the production of Castelli ceramics and presents first archaeometric data on the maiolica production from Ascoli Piceno. The scientific examination highlights continuity with the Renaissance production, and the joint contribution of the three analytical techniques suggests distinctive features among different productions, thus integrating and refining the information obtained by the art-historical study.

Structure of a radiate pseudocolony associated with an intrauterine contraceptive device

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

O'Brien, P.K.; Lea, P.J.; Roth-Moyo, L.A.

Transmission electron microscopy of a radiate pseudocolony associated with an intrauterine contraceptive device (IUCD) showed central bundles of extracellular fibers averaging 35 nm in diameter, surrounded by layered mantles of electron-dense, amorphous granular material. No bacterial, viral, or fungal structures were present. X-ray microanalysis revealed copper, sulfur, chloride, iron, and phosphorus; no calcium was found. It is postulated that these structures and histologically identical non-IUCD-associated granules from the female genital tract, as well as similar structures from other body locations, including those reported in colloid cysts of the third ventricle, are of lipofuscin origin.

Electrodeposition of thin yttria-stabilized zirconia layers using glow-discharge plasma

NASA Astrophysics Data System (ADS)

Ogumi, Zempachi; Uchimoto, Yoshiharu; Tsuji, Yoichiro; Takehara, Zen-ichiro

1992-08-01

A novel process for preparation of thin yttria-stabilized zirconia (YSZ) layers was developed. This process differs from other vapor-phase deposition methods in that a dc bias circuit, separate from the plasma-generation circuit, is used for the electrodeposition process. The YSZ layer was electrodeposited from ZrCl4 and YCl3 on a nonporous calcia-stabilized zirconia substrate. Scanning electron microscopy, electron probe microanalysis, electron spectroscopy for chemical analysis, and x-ray-diffraction measurements confirmed the electrodeposition of a smooth, pinhole-free yttria-stabilized zirconia film of about 3 μm thickness.

Identification of stainless steel welding fume particulates in human lung and environmental samples using electron probe microanalysis.

PubMed

Stettler, L E; Groth, D H; MacKay, G R

1977-02-01

Open lung biopsy specimens from two welders and air samples from their workplace environments were examined with the electron probe microanalyzer. X-ray analysis showed that the majority of particles found in the lung tissue from both workers and in the air samples to be composed of varying amounts of iron, chromium, manganese and nickel, the major components of some types of stainless steel. Based upon these analyses, it was concluded that the majority of the particles in both biopsy specimens were a result of the workplace environment.

Secondary sulfate minerals from Alum Cave Bluff: Microscopy and microanalysis

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

Lauf, R.J.

1997-07-01

Microcrystals of secondary sulfate minerals from Alum Cave Bluff, Great Smoky Mountains National Park, were examined by scanning electron microscopy and identified by X-ray fluorescence (XRF) in the SEM. Among the samples the author discovered three new rare-earth sulfates: coskrenite-(Ce), levinsonite-(Y), and zugshunstite-(Ce). Other minerals illustrated in this report include sulfur, tschermigite, gypsum, epsomite, melanterite, halotrichite, apjohnite, jarosite, slavikite, magnesiocopiapite, and diadochite. Additional specimens whose identification is more tentative include pickeringite, aluminite, basaluminite, and botryogen. Alum Cave is a ``Dana locality`` for apjohnite and potash alum, and is the first documented North American occurrence of slavikite.

Analysis of pigments from Roman wall paintings found in the "agro centuriato" of Julia Concordia (Italy).

PubMed

Mazzocchin, Gian-Antonio; Del Favero, Michela; Tasca, Giovanni

2007-09-01

The analysis of wall painting fragments recovered in the "agro centuriato" of Julia Concordia has been carried out by using Scanning Electron Microscopy equipped with an EDS microanalysis detector (SEM-EDS), Infrared Spectroscopy (FTIR) and X-Ray powder Diffraction (XRD). The pigments used have been identified and the data obtained suggest the presence of three rustic villas richly decorated also with Egyptian blue. The presence of white of aragonite suggest that these villas were decorated during the Imperial Age, in agreement with the recovery of high quality materials and a bronze statue.

Application of micro-Fourier transform infrared spectroscopy to the examination of paint samples

NASA Astrophysics Data System (ADS)

Zięba-Palus, J.

1999-11-01

The examination and identification of automobile paints is an important problem in road accidents investigations. Since the real sample available is very small, only sensitive microtechniques can be applied. The methods of optical microscopy and micro-Fourier transform infrared spectroscopy (MK-FTIR) supported by scanning electron microscopy together with X-ray microanalysis (SEM-EDX) allow one to carry out the examination of each paint layer without any separation procedure. In this paper an attempt is made to discriminate between different automobile paints of the same colour by the use of these methods for criminalistic investigations.

Bladder stone in a human female: The case of an abnormally located intrauterine contraceptive device

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

Khan, S.R.; Wilkinson, E.J.

A single 4.7 x 3.3 x 1.5 cm solid nodule was removed from the bladder of a 24 years old white female who had lost an intrauterine contraceptive device (IUD) installed approximately four years ago. The nodule showed no external evidence of an IUD or its string. An examination of the nodular surface by scanning electron microscopy (SEM) showed mostly amorphous material with some adherent filamentous structures. Its energy dispersive x-ray microanalysis revealed the presence of calcium and phosphorus suggesting that the nodule was actually a urolith. Fracturing the nodule exposed an embedded entity consistent with being a copper IUD.more » Apparently, the lost IUD had migrated from the uterus into the bladder where it became mineralized. Thus the solid nodule was actually a foreign body stone.« less

Single-particle characterization of atmospheric aerosols collected at Gosan, Korea, during the Asian Pacific Regional Aerosol Characterization Experiment field campaign using low-Z (atomic number) particle electron probe X-ray microanalysis.

PubMed

Geng, Hong; Cheng, Fangqin; Ro, Chul-Un

2011-11-01

A quantitative energy-dispersive electron probe X-ray microanalysis (ED-EPMA), namely low-Z (atomic number) particle EPMA, was used to characterize the chemical compositions of the individual aerosol particles collected at the Gosan supersite, Jeju Island, Korea, as a part of the Asian Pacific Regional Aerosol Characterization Experiment (ACE-Asia). On 4-10 April 2001 just before a severe dust storm arrived, seven sets of aerosol samples were obtained by a seven-stage May cascade impactor with a flow rate of 20 L/min. Overall 11,200 particles on stages 1-6 with cutoff diameters of 16, 8, 4, 2, 1, and 0.5 microm, respectively, were examined and classified based on their secondary electron images and X-ray spectra. In general, sea salt particles were the most frequently encountered, followed by mineral dust, organic carbon (OC)-like, (NH4)2SO4/NH4HSO4-containing, elemental carbon (EC)-like, Fe-rich, and K-rich particles. Sea salt and mineral dust particles had a higher relative abundance on stages 1-5, whereas OC-like, (NH4)2SO4/NH4HSO4-containing, Fe-rich, and K-rich particles were relatively abundant on stage 6. The analysis on relative number abundances of various particle types combined with 72-hr backward air mass trajectories indicated that a lot of reacted sea salt and reacted mineral dust (with airborne NOx and SO2 or their acidic products) and OC-like particles were carried by the air masses passing over the Yellow Sea (for sample "10 April") and many NH4HSO4/ (NH4)2SO4-containing particles were carried by the air masses passing over the Sea of Japan and Korea Strait (for samples "4-9 April"). It was concluded that the atmosphere over Jeju Island was influenced by anthropogenic SO2 and NOx, organic compounds, and secondary aerosols when Asian dust was absent.

Observational techniques for solar flare gamma-rays, hard X-rays, and neutrons

NASA Technical Reports Server (NTRS)

Lin, Robert P.

1989-01-01

The development of new instrumentation and techniques for solar hard X-ray, gamma ray and neutron observations from spacecraft and/or balloon-borne platforms is examined. The principal accomplishments are: (1) the development of a two segment germanium detector which is near ideal for solar hard X-ray and gamma ray spectroscopy; (2) the development of long duration balloon flight techniques and associated instrumentation; and (3) the development of innovative new position sensitive detectors for hard X-ray and gamma rays.

Study on the surface sulfidization behavior of smithsonite at high temperature

NASA Astrophysics Data System (ADS)

Lv, Jin-fang; Tong, Xiong; Zheng, Yong-xing; Xie, Xian; Wang, Cong-bing

2018-04-01

Surface sulfidization behavior of smithsonite at high temperature was investigated by X-ray powder diffractometer (XRD) along with thermodynamic calculation, X-ray photoelectron spectroscopy (XPS) and electron probe microanalysis (EPMA). The XRD and thermodynamic analyses indicated that the smithsonite was decomposed into zincite at high temperatures. After introducing a small amount of pyrite, artificial sulfides were formed at surface of the obtained zincite. The XPS analyses revealed that the sulfide species including zinc sulfide and zinc disulfide were generated at the zincite surface. The EPMA analyses demonstrated that the film of sulfides was unevenly distributed at the zincite surface. The average concentration of elemental sulfur at the sample surface increased with increasing of pyrite dosage. A suitable mole ratio of FeS2 to ZnCO3 for the surface thermal modification was determined to be about 0.3. These findings can provide theoretical support for improving the process during which the zinc recovery from refractory zinc oxide ores is achieved by xanthate flotation.

Growth and structural, optical, and electrical properties of zincite crystals

NASA Astrophysics Data System (ADS)

Kaurova, I. A.; Kuz'micheva, G. M.; Rybakov, V. B.

2013-03-01

An X-ray diffraction study of ZnO crystals grown by the hydrothermal method has revealed reflections that give grounds to assign them to the sp. gr. P3 rather than to P63 mc. The distribution of Zn1, Zn2, O1, and O2 over structural positions, along with vacancies and incorporated zinc atoms, explains the dissymmetrization observed in terms of the kinetic (growth) phase transition of the order-disorder type, which is caused by ordering Zn and O atoms over structural positions. The color of crystals of refined compositions (Zn0.975□0.025)Zn i(0.015)(O0.990□0.010) (green) and (Zn0.965□0.035)Zn i(0.035)O (bright green) is related to different oxygen contents, which is confirmed by the results of electron probe X-ray microanalysis and absorption spectroscopy. The degree of the structural quality of crystals, their resistivity, and activation energy are also related to oxygen vacancies.

Influence of microstructure on hardness of plasma sprayed Al2O3-TiO2-MgO coatings with interface diffusion by heat treatment

NASA Astrophysics Data System (ADS)

Chen, Kunlun; Song, Peng; Li, Chao; Lu, Jiansheng

2017-12-01

The effect of heat treatment on the microstructure and mechanical properties of Al2O3-TiO2 coatings doped with 5 wt% MgO was investigated in this paper. The composite coatings were prepared by atmospheric plasma spraying (APS) and heat treated at 1000 °C for 24 h in Ar. The coatings were analyzed using scanning electron microscopy with electron probe x-ray microanalysis and x-ray diffraction. The hardness was determined using a Vickers hardness test on the as-sprayed coatings and after heat treatment. The results showed that the interface diffusion between the Al-rich and Ti-rich layers resulted in mutual pinning within the coating during the heat treatment. The newly formed MgAl2O4 phase promoted cracking-healing behavior within the coating. We conclude that increase of the hardness of the coatings was mainly caused by the mutual pinning interface and crack healing.

Ultrastructural and elemental analysis of sialoliths and their comparison with nephroliths.

PubMed

Rakesh, Nagaraju; Bhoomareddy Kantharaj, Yashoda Devi; Agarwal, Manjushree; Agarwal, Kunal

2014-02-01

Sialoliths are common in the submandibular gland and its duct system, although their exact cause of formation is still a matter of debate. The aims of this study were to: (a) analyze sialoliths ultrastructurally, and to determine the role of foreign bodies or organic materials in the formation of sialolith nuclei; and (b) compare nephroliths with sialoliths ultrastructurally. Three sialoliths and two nephroliths were analyzed ultrastructurally by a scanning electron microscope and X-ray diffractometer. The main structures of the sialoliths were found to be hydroxyapatite crystals. No organic cores were observed in the central parts of the sialoliths. In nephroliths, calcium oxalate, calcium phosphate, and struvite crystals were found. The energy-dispersive X-ray microanalysis found that sialoliths and nephroliths were predominantly composed of elements comprising calcium, phosphorous, magnesium, sodium, chloride, silicon, iron, and potassium. Sialoliths in the submandibular salivary glands might form secondary to sialadenitis, but not via a luminal organic nidus. © 2014 Wiley Publishing Asia Pty Ltd.

Advanced Microstructural Study of Suspension Plasma Sprayed Hydroxyapatite Coatings

NASA Astrophysics Data System (ADS)

Podlesak, Harry; Pawlowski, Lech; D'Haese, Romain; Laureyns, Jacky; Lampke, Thomas; Bellayer, Severine

2010-03-01

Fine, home-synthesized, hydroxyapatite powder was formulated with water and alcohol to obtain a suspension used to plasma spray coatings onto a titanium substrate. The deposition process was optimized using statistical design of 2 n experiments with two variables: spray distance and electric power input to plasma. X-ray diffraction (XRD) was used to determine quantitatively the phase composition of obtained deposits. Raman microscopy and electron probe microanalysis (EPMA) enabled localization of the phases in different positions of the coating cross sections. Transmission electron microscopic (TEM) study associated with energy-dispersive x-ray spectroscopy (EDS) enabled visualization and analysis of a two-zone microstructure. One zone contained crystals of hydroxyapatite, tetracalcium phosphate, and a phase rich in calcium oxide. This zone included lamellas, usually observed in thermally sprayed coatings. The other zone contained fine hydroxyapatite grains that correspond to nanometric and submicrometric solids from the suspension that were agglomerated and sintered in the cold regions of plasma jet and on the substrate.

Analysis of the Henze precipitate from the blood cells of the ascidian Phallusia mammillata

NASA Astrophysics Data System (ADS)

Ciancio, Aurelio; Scippa, Silvia; Nette, Geoffrey; De Vincentiis, Mario

The Henze precipitate, a peculiar blue-green microparticulate obtained by lysis of the blood cells of the ascidian Phallusia mammillata (Protochordata), was investigated with atomic force microscopy (AFM), scanning electron microscopy (SEM) and X-ray microanalysis. The precipitate was collected from the Henze solution, an unstable red-brown product obtained by treating blood with distilled water, whose degradation yields a characteristic blue-green product. The microparticulates measured 50-100 µm in diameter and appeared irregular in shape. SEM examination showed smooth, roughly round boundaries. The microparticulate surface examined with AFM appeared as an irregular matrix formed by 70-320-nm-wide mammillate composites, including and embedding small (500-800 nm wide) crystal-like multilayered formations. X- ray analysis showed that the elements present in these same precipitates were mainly C, Si, Al and O. The microparticulate composition appeared close to those of natural waxes or lacquers, embedding amorphous silicates and/or other Si-Al components. The unusual occurrence of Si in ascidian blood and its role are discussed.

Formation of Porous Germanium Layers by Silver-Ion Implantation

NASA Astrophysics Data System (ADS)

Stepanov, A. L.; Vorob'ev, V. V.; Nuzhdin, V. I.; Valeev, V. F.; Osin, Yu. N.

2018-04-01

We propose a method for the formation of porous germanium ( P-Ge) layers containing silver nanoparticles by means of high-dose implantation of low-energy Ag+ ions into single-crystalline germanium ( c-Ge). This is demonstrated by implantation of 30-keV Ag+ ions into a polished c-Ge plate to a dose of 1.5 × 1017 ion/cm2 at an ion beam-current density of 5 μA/cm2. Examination by high-resolution scanning electron microscopy (SEM), atomic-force microscopy (AFM), X-ray diffraction (XRD), energy-dispersive X-ray (EDX) microanalysis, and reflection high-energy electron diffraction (RHEED) showed that the implantation of silver ions into c-Ge surface led to the formation of a P-Ge layer with spongy structure comprising a network of interwoven nanofibers with an average diameter of ˜10-20 nm Ag nanoparticles on the ends of fibers. It is also established that the formation of pores during Ag+ ion implantation is accompanied by effective sputtering of the Ge surface.

Corrosion behavior of low alloy steels in a wet-dry acid humid environment

NASA Astrophysics Data System (ADS)

Zhao, Qing-he; Liu, Wei; Yang, Jian-wei; Zhu, Yi-chun; Zhang, Bin-li; Lu, Min-xu

2016-09-01

The corrosion behavior of corrosion resistant steel (CRS) in a simulated wet-dry acid humid environment was investigated and compared with carbon steel (CS) using corrosion loss, polarization curves, X-ray diffraction (XRD), scanning electron microscopy (SEM), electron probe micro-analysis (EPMA), N2 adsorption, and X-ray photoelectron spectroscopy (XPS). The results show that the corrosion kinetics of both steels were closely related to the composition and compactness of the rust, and the electrochemical properties of rusted steel. Small amounts of Cu, Cr, and Ni in CRS increased the amount of amorphous phases and decreased the content of γ-FeOOH in the rust, resulting in higher compactness and electrochemical stability of the CRS rust. The elements Cu, Cr, and Ni were uniformly distributed in the CRS rust and formed CuFeO2, Cu2O, CrOOH, NiFe2O4, and Ni2O3, which enhanced the corrosion resistance of CRS in the wet-dry acid humid environment.

Electron microprobe analysis and histochemical examination of the calcium distribution in human bone trabeculae: a methodological study using biopsy specimens from post-traumatic osteopenia

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

Obrant, K.J.; Odselius, R.

1984-01-01

Energy dispersive X-ray microanalysis (EDX) (or electron microprobe analysis) of the relative intensity for calcium in different bone trabeculae from the tibia epiphysis, and in different parts of one and the same trabecula, was performed on 3 patients who had earlier had a fracture of the ipsilateral tibia-diaphysis. The variation in intensity was compared with the histochemical patterns obtained with both the Goldner and the von Kossa staining techniques for detecting calcium in tissues. Previously reported calcium distribution features, found to be typical for posttraumatic osteopenia, such as striated mineralization patterns in individual trabeculae and large differences in mineralization levelmore » between different trabeculae, could be verified both by means of the two histochemical procedures and from the electron microprobe analysis. A pronounced difference was observed, however, between the two histochemical staining techniques as regards their sensitivity to detect calcium. To judge from the values obtained from the EDX measurements, the sensitivity of the Goldner technique should be more than ten times higher than that of von Kossa. The EDX measurements gave more detailed information than either of the two histochemical techniques: great variations in the intensity of the calcium peak were found in trabeculae stained as unmineralized as well as mineralized.« less

Synchrotron applications in wood preservation and deterioration

Treesearch

Barbara L. Illman

2003-01-01

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

Today's and Tomorrow's Instruments.

PubMed

Conty, Claude

2001-03-01

This article will discuss the importance of Raimond Castaing's thesis on the genesis of a nondestructive and truly quantitative microanalytical method that assisted the scientific community in moving forward in the development of microanalytical instruments. I will also share with you my recollection of the decades of improvement in the electron probe microanalyzer (EPMA), that has allowed us to reach our present level of instrument sophistication, and I will explore with you my thoughts on the future evolution of this technique. To conclude, I will present the current status of related microanalysis techniques developed under Castaing in Orsay in the 1960s, as Castaing's interest in microanalysis was not limited to electron probe microanalysis alone.

TOPICAL REVIEW: Human soft tissue analysis using x-ray or gamma-ray techniques

NASA Astrophysics Data System (ADS)

Theodorakou, C.; Farquharson, M. J.

2008-06-01

This topical review is intended to describe the x-ray techniques used for human soft tissue analysis. X-ray techniques have been applied to human soft tissue characterization and interesting results have been presented over the last few decades. The motivation behind such studies is to provide improved patient outcome by using the data obtained to better understand a disease process and improve diagnosis. An overview of theoretical background as well as a complete set of references is presented. For each study, a brief summary of the methodology and results is given. The x-ray techniques include x-ray diffraction, x-ray fluorescence, Compton scattering, Compton to coherent scattering ratio and attenuation measurements. The soft tissues that have been classified using x-rays or gamma rays include brain, breast, colon, fat, kidney, liver, lung, muscle, prostate, skin, thyroid and uterus.

Application of Quantitative Analytical Electron Microscopy to the Mineral Content of Insect Cuticle

NASA Astrophysics Data System (ADS)

Rasch, Ron; Cribb, Bronwen W.; Barry, John; Palmer, Christopher M.

2003-04-01

Quantification of calcium in the cuticle of the fly larva Exeretonevra angustifrons was undertaken at the micron scale using wavelength dispersive X-ray microanalysis, analytical standards, and a full matrix correction. Calcium and phosphorus were found to be present in the exoskeleton in a ratio that indicates amorphous calcium phosphate. This was confirmed through electron diffraction of the calcium-containing tissue. Due to the pragmatic difficulties of measuring light elements, it is not uncommon in the field of entomology to neglect the use of matrix corrections when performing microanalysis of bulk insect specimens. To determine, firstly, whether such a strategy affects the outcome and secondly, which matrix correction is preferable, phi-rho (z) and ZAF matrix corrections were contrasted with each other and without matrix correction. The best estimate of the mineral phase was found to be given by using the phi-rho (z) correction. When no correction was made, the ratio of Ca to P fell outside the range for amorphous calcium phosphate, possibly leading to flawed interpretation of the mineral form when used on its own.

Preparation of a Ytterbium-tagged Gunshot Residue Standard for Quality Control in the Forensic Analysis of GSR.

PubMed

Hearns, Nigel G R; Laflèche, Denis N; Sandercock, Mark L

2015-05-01

Preparation of a ytterbium-tagged gunshot residue (GSR) reference standard for scanning electron microscopy and energy dispersive X-ray spectroscopic (SEM-EDS) microanalysis is reported. Two different chemical markers, ytterbium and neodymium, were evaluated by spiking the primers of 38 Special ammunition cartridges (no propellant, no projectile) and discharging them onto 12.7 mm diameter aluminum SEM pin stubs. Following SEM-EDS microanalysis, the majority of tri-component particles containing lead, barium, and antimony (PbBaSb) were successfully tagged with the chemical marker. Results demonstrate a primer spiked with 0.75% weight percent of ytterbium nitrate affords PbBaSb particles characteristic of GSR with a ytterbium inclusion efficiency of between 77% and 100%. Reproducibility of the method was verified, and durability of the ytterbium-tagged tri-component particles under repeated SEM-EDS analysis was also tested. The ytterbium-tagged PbBaSb particles impart synthetic traceability to a GSR reference standard and are suitable for analysis alongside case work samples, as a positive control for quality assurance purposes. © 2015 American Academy of Forensic Sciences.

Blue light-dependent changes in loosely bound calcium in Arabidopsis mesophyll cells: an X-ray microanalysis study.

PubMed

Łabuz, Justyna; Samardakiewicz, Sławomir; Hermanowicz, Paweł; Wyroba, Elżbieta; Pilarska, Maria; Gabryś, Halina

2016-06-01

Calcium is involved in the signal transduction pathway from phototropins, the blue light photoreceptor kinases which mediate chloroplast movements. The chloroplast accumulation response in low light is controlled by both phot1 and phot2, while only phot2 is involved in avoidance movement induced by strong light. Phototropins elevate cytosolic Ca(2+) after activation by blue light. In higher plants, both types of chloroplast responses depend on Ca(2+), and internal calcium stores seem to be crucial for these processes. Yet, the calcium signatures generated after the perception of blue light by phototropins are not well understood. To characterize the localization of calcium in Arabidopsis mesophyll cells, loosely bound (exchangeable) Ca(2+) was precipitated with potassium pyroantimonate and analyzed by transmission electron microscopy followed by energy-dispersive X-ray microanalysis. In dark-adapted wild-type Arabidopsis leaves, calcium precipitates were observed at the cell wall, where they formed spherical structures. After strong blue light irradiation, calcium at the apoplast prevailed, and bigger, multilayer precipitates were found. Spherical calcium precipitates were also detected at the tonoplast. After red light treatment as a control, the precipitates at the cell wall were smaller and less numerous. In the phot2 and phot1phot2 mutants, calcium patterns were different from those of wild-type plants. In both mutants, no elevation of calcium after blue light treatment was observed at the cell periphery (including the cell wall and a fragment of cytoplasm). This result confirms the involvement of phototropin2 in the regulation of Ca(2+) homeostasis in mesophyll cells. © The Author 2016. Published by Oxford University Press on behalf of the Society for Experimental Biology.

Intracellular ion concentrations and cell volume during cholinergic stimulation of eccrine secretory coil cells

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

Takemura, T.; Sato, F.; Saga, K.

Methacholine (MCh)-induced changes in intracellular concentrations of Na, K, and Cl (( Na)i, (K)i, and (Cl)i, respectively) and in cellular dry mass (a measure of cell shrinkage) were examined in isolated monkey eccrine sweat secretory coils by electron probe X-ray microanalysis using the peripheral standard method. To further confirm the occurrence of cell shrinkage during MCh stimulation, the change in cell volume of dissociated clear and dark cells were directly determined under a light microscope equipped with differential interference contrast (DIC) optics. X-ray microanalysis revealed a biphasic increase in cellular dry mass in clear cells during continuous MCh stimulation; anmore » initial increase of dry mass to 158% (of control) followed by a plateau at 140%, which correspond to the decrease in cell volume of 37 and 29%, respectively. The latter agrees with the MCh-induced cell shrinkage of 29% in dissociated clear cells. The MCh-induced increase in dry mass in myoepithelial cells was less than half that of clear cells. During the steady state of MCh stimulation, both (K+)i and (Cl)i of clear cells decreased by about 45%, whereas (Na)i increased in such a way to maintain the sum of (Na) i + (K)i constant. There was a small (12-15 mM) increase in (Na)i and a decrease in (K)i in myoepithelial cells during stimulation with MCh. Dissociated dark cells failed to significantly shrink during MCh stimulation. The decrease in (Cl)i in the face of constant (Na)i + (K)i suggests the accumulation of unknown anion(s) inside the clear cell during MCh stimulation.« less

Tribological properties of TiC/a-C:H nanocomposite coatings prepared via HiPIMS

NASA Astrophysics Data System (ADS)

Sánchez-López, J. C.; Dominguez-Meister, S.; Rojas, T. C.; Colasuonno, M.; Bazzan, M.; Patelli, A.

2018-05-01

High power impulse magnetron sputtering (HiPIMS) technology has been employed to prepare TiC/a-C:H nanocomposite coatings from a titanium target in acetylene (C2H2) reactive atmospheres. Gas fluxes were varied from 1.3 to 4.4 sccm to obtain C/Ti ratios from 2 to 15 as measured by electron probe microanalysis (EPMA). X-ray diffraction and transmission electron microscopy demonstrate the presence of TiC nanocrystals embedded in an amorphous carbon-based matrix. The hardness properties decrease from 17 to 10 GPa as the carbon content increases. The tribological properties were measured using a pin-on-disk tribometer in ambient air (RH = 30-40%) at 10 cm/s with 5 N of applied load against 6-mm 100Cr6 balls. The friction coefficient and the film wear rates are gradually improved from 0.3 and 7 × 10-6 mm3/N m to 0.15 and 2 × 10-7 mm3/N m, respectively, by increasing the C2H2 flux. To understand the tribological processes appearing at the interface and to elucidate the wear mechanism, microstructural and chemical investigations of the coatings were performed before and after the friction test. EPMA, X-ray photoelectron and electron energy-loss spectroscopies were employed to obtain an estimation of the fraction of the a-C:H phase, which can be correlated with the tribological behavior. Examination of the friction counterfaces (ball and track) by Raman microanalysis reveals an increased ordering of the amorphous carbon phase concomitant with friction reduction. The tribological results were compared with similar TiC/a-C(:H) composites prepared by the conventional direct current process.

Pulsed electrodeposition for the synthesis of strontium-substituted calcium phosphate coatings with improved dissolution properties.

PubMed

Drevet, Richard; Benhayoune, Hicham

2013-10-01

Strontium-substituted calcium phosphate coatings are synthesized by pulsed electrodeposition on titanium alloy (Ti6Al4V) substrates. Experimental conditions of the process are optimized in order to obtain a coating with a 5% atomic substitution of calcium by strontium which corresponds to the best observations on the osteoblast cells activity and on the osteoclast cells proliferation. The physical and chemical characterizations of the obtained coating are carried out by scanning electron microscopy associated to energy dispersive X-ray spectroscopy (EDXS) for X-ray microanalysis and the structural characterization of the coating is carried out by X-ray diffraction. The in vitro dissolution/precipitation properties of the coated substrates are investigated by immersion into Dulbecco's Modified Eagle Medium (DMEM) from 1h to 14 days. The calcium, phosphorus and strontium concentrations variations in the biological liquid are assessed by Induced Coupled Plasma - Atomic Emission Spectroscopy for each immersion time. The results show that under specific experimental conditions, the electrodeposition process is suitable to synthesize strontium-substituted calcium phosphate coatings. Moreover, the addition of hydrogen peroxide (H2O2) into the electrolytic solution used in the process allows us to observe a control of the strontium release during the immersion of the prosthetic materials into DMEM. © 2013.

Effect of UV-ozone treatment on poly(dimethylsiloxane) membranes: surface characterization and gas separation performance.

PubMed

Fu, Ywu-Jang; Qui, Hsuan-zhi; Liao, Kuo-Sung; Lue, Shingjiang Jessie; Hu, Chien-Chieh; Lee, Kueir-Rarn; Lai, Juin-Yih

2010-03-16

A thin SiO(x) selective surface layer was formed on a series of cross-linked poly(dimethylsiloxane) (PDMS) membranes by exposure to ultraviolet light at room temperature in the presence of ozone. The conversion of the cross-linked polysiloxane to SiO(x) was monitored by attenuated total reflectance Fourier transform infrared (ATR-FTIR) spectroscopy, X-ray photoelectron spectroscopy (XPS), energy-dispersive X-ray (EDX) microanalysis, contact angle analysis, and atomic force microscopy (AFM). The conversion of the cross-linked polysiloxane to SiO(x) increased with UV-ozone exposure time and cross-linking agent content, and the surface possesses highest conversion. The formation of a SiO(x) layer increased surface roughness, but it decreased water contact angle. Gas permeation measurements on the UV-ozone exposure PDMS membranes documented interesting gas separation properties: the O(2) permeability of the cross-linked PDMS membrane before UV-ozone exposure was 777 barrer, and the O(2)/N(2) selectivity was 1.9; after UV-ozone exposure, the permeability decreased to 127 barrer while the selectivity increased to 5.4. The free volume depth profile of the SiO(x) layer was investigated by novel slow positron beam. The results show that free volume size increased with the depth, yet the degree of siloxane conversion to SiO(x) does not affect the amount of free volume.

Gold coated copper artifacts from the Royal Tombs of Sipán (Huaca Rajada, Perù): manufacturing techniques and corrosion phenomena

NASA Astrophysics Data System (ADS)

Ingo, Gabriel M.; Bustamante, Angel D.; Alva, Walter; Angelini, Emma; Cesareo, Roberto; Gigante, Giovanni E.; Zambrano, Sandra Del Pilar A.; Riccucci, Cristina; Di Carlo, Gabriella; Parisi, Erica I.; Faraldi, Federica; Chero, Luis; Fabian, Julio S.

2013-12-01

Twenty five years ago, close to the northern Peruvian town of Lambayeque (Huaca Rajada) beneath two large and eroded pyramids, built of adobe mud bricks, Professor Alva discovered the world-famous unlooted pre-Columbian burial chambers of the Royal Tombs of Sipan. The tombs contained a large amount of objects of exceptional artistic and historical value including the greatest intact number of gold and silver artefacts in the Americas to be considered one of the most important archaeological discoveries of the last century. Some copper based objects coated with thin layers of gold have been studied by means of the combined use of analytical techniques such as optical microscopy (OM), scanning electron microscopy coupled with energy dispersive X-ray micro-analysis (SEM-EDS), X-ray photoelectron spectroscopy (XPS), and X-ray diffraction (XRD) in order to identify the chemical composition and the manufacturing processes of the gold layer as well as the corrosion products formed during the long-term burial. The micro-chemical and structural results give useful information about the manufacturing techniques used by the Moche metalsmiths to modify the surface chemical composition of the coated artefacts likely based on the depletion gilding process carried out by oxidising the surface copper containing the noble metal and etching away the copper oxides. Furthermore, the results reveal that the main degradation agent is the ubiquitous chlorine and that copper has been almost completely transformed during the burial into mineral species giving rise to the formation of stratified structures constituted by different mineral phases such as cuprous oxide (Cu2O) and copper carbonates [azurite (Cu3(CO3)2(OH)2 and malachite (CuCO3Cu(OH)2)] as well as dangerous chlorine-based compounds such as nantokite (CuCl) and atacamite (Cu2(OH)3Cl) polymorphs. These information evidence the strict interaction of the alloying elements with the soil components as well as the occurrence of the copper cyclic corrosion as post-burial degradation phenomenon. The present study confirms that the combined use of micro-chemical and micro-structural investigation techniques such as SEM-EDS, XPS, XRD, and OM can be successfully used to investigate the technological manufacturing processes of the ancient coated artefacts and to achieve information about degradation agents and mechanisms useful to define tailored conservation strategies possibly including new, more reliable, and safer materials.

Potential for Imaging Engineered Tissues with X-Ray Phase Contrast

PubMed Central

Appel, Alyssa; Anastasio, Mark A.

2011-01-01

As the field of tissue engineering advances, it is crucial to develop imaging methods capable of providing detailed three-dimensional information on tissue structure. X-ray imaging techniques based on phase-contrast (PC) have great potential for a number of biomedical applications due to their ability to provide information about soft tissue structure without exogenous contrast agents. X-ray PC techniques retain the excellent spatial resolution, tissue penetration, and calcified tissue contrast of conventional X-ray techniques while providing drastically improved imaging of soft tissue and biomaterials. This suggests that X-ray PC techniques are very promising for evaluation of engineered tissues. In this review, four different implementations of X-ray PC imaging are described and applications to tissues of relevance to tissue engineering reviewed. In addition, recent applications of X-ray PC to the evaluation of biomaterial scaffolds and engineered tissues are presented and areas for further development and application of these techniques are discussed. Imaging techniques based on X-ray PC have significant potential for improving our ability to image and characterize engineered tissues, and their continued development and optimization could have significant impact on the field of tissue engineering. PMID:21682604

Synthesis and characterization of a pH-sensitive conjugate of isoniazid with Fe3O4@SiO2 magnetic nanoparticles.

PubMed

Sedlák, Miloš; Bhosale, Dattatry Shivajirao; Beneš, Ludvík; Palarčík, Jiří; Kalendová, Andrea; Královec, Karel; Imramovský, Aleš

2013-08-15

The Letter describes the preparation and characterization of a conjugate of isoniazid (INH) with magnetic nanoparticles Fe3O4@SiO2 115±60 nm in size. The INH molecules were attached to the surface of nanoparticles by a covalent pH-sensitive amidine bond. The conjugate was characterized by X-ray diffraction, SEM, dynamic light scattering, IR spectroscopy and microanalysis. The conjugate released isoniazid under in vitro conditions (pH=4; 37 °C; t1/2≈115 s). In addition, the cytotoxicity of the Fe3O4@SiO2-INH conjugate was evaluated in SK-BR-3 cells using the xCELLigence system. Copyright © 2013 Elsevier Ltd. All rights reserved.

Kinetics of heterogeneous reaction of CaCO3 particles with gaseous HNO3 over a wide range of humidity.

PubMed

Liu, Y; Gibson, E R; Cain, J P; Wang, H; Grassian, V H; Laskin, A

2008-02-21

Heterogeneous reaction kinetics of gaseous nitric acid (HNO3) with calcium carbonate (CaCO3) particles was investigated using a particle-on-substrate stagnation flow reactor (PS-SFR). This technique utilizes the exposure of substrate deposited, isolated, and narrowly dispersed particles to a gas mixture of HNO3/H2O/N2, followed by microanalysis of individual reacted particles using computer-controlled scanning electron microscopy with energy-dispersive X-ray analysis (CCSEM/EDX). The first series of experiments were conducted at atmospheric pressure, room temperature and constant relative humidity (40%) with a median dry particle diameter of Dp = 0.85 mum, particle loading densities 2 x 104 /= 0.06 (x3//2). In a second series of experiments, HNO3 uptake on CaCO3 particles of the same size was examined over a wide range of relative humidity, from 10 to 80%. The net reaction probability was found to increase with increasing relative humidity, from gammanet >/= 0.003 at RH = 10% to 0.21 at 80%.

Taguchi's technique: an effective method for improving X-ray medical radiographic screen performance.

PubMed

Vlachogiannis, J G

2003-01-01

Taguchi's technique is a helpful tool to achieve experimental optimization of a large number of decision variables with a small number of off-line experiments. The technique appears to be an ideal tool for improving the performance of X-ray medical radiographic screens under a noise source. Currently there are very many guides available for improving the efficiency of X-ray medical radiographic screens. These guides can be refined using a second-stage parameter optimization. based on Taguchi's technique, selecting the optimum levels of controllable X-ray radiographic screen factors. A real example of the proposed technique is presented giving certain performance criteria. The present research proposes the reinforcement of X-ray radiography by Taguchi's technique as a novel hardware mechanism.

Coherent X-ray imaging across length scales

NASA Astrophysics Data System (ADS)

Munro, P. R. T.

2017-04-01

Contemporary X-ray imaging techniques span a uniquely wide range of spatial resolutions, covering five orders of magnitude. The evolution of X-ray sources, from the earliest laboratory sources through to highly brilliant and coherent free-electron lasers, has been key to the development of these imaging techniques. This review surveys the predominant coherent X-ray imaging techniques with fields of view ranging from that of entire biological organs, down to that of biomolecules. We introduce the fundamental principles necessary to understand the image formation for each technique as well as briefly reviewing coherent X-ray source development. We present example images acquired using a selection of techniques, by leaders in the field.

Structural and phase transformation of A{sup III}B{sup V}(100) semiconductor surface in interaction with selenium

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

Bezryadin, N. N.; Kotov, G. I., E-mail: giktv@mail.ru; Kuzubov, S. V., E-mail: kuzub@land.ru

2015-03-15

Surfaces of GaAs(100), InAs(100), and GaP(100) substrates thermally treated in selenium vapor have been investigated by transmission electron microscopy and electron probe X-ray microanalysis. Some specific features and regularities of the formation of A{sub 3}{sup III}B{sub 4}{sup VI} (100)c(2 × 2) surface phases and thin layers of gallium or indium selenides A{sub 2}{sup III}B{sub 3}{sup VI} (100) on surfaces of different A{sup III}B{sup V}(100) semiconductors are discussed within the vacancy model of surface atomic structure.

Correlation between impurity distribution and location of ferroelectric domain walls in Nd : Mg : LiNbO 3 single crystal

NASA Astrophysics Data System (ADS)

Naumova, I. I.; Evlanova, N. F.; Blokhin, S. A.; Lavrishchev, S. V.

1998-04-01

Using selective chemical etching, scanning electron microscope (SEM) and wave dispersive X-ray (WDX) microanalysis we showed that the ferroelectric domain walls coincide with the maxima and minima Nd-impurity modulation in a periodically poled Nd : Mg : LiNbO 3 crystal grown by the Czochralski method along the normal to the (0 1 1¯ 2) face. Asymmetric form of the Nd-modulation produces nonequal positive and negative domains for one period. Variations of instantaneous rate of growth were estimated for facet and nonfacet crystal region in the framework of Burton-Prim-Slichter theory.

Ion transport across the exocrine glands of the frog skin.

PubMed

Mills, J W

1985-01-01

Exposure of the intact frog skin to beta-adrenergic agonists stimulates chloride secretion by the exocrine glands. The secretory response is dependent on Na in the serosal bath and is inhibited by exposure to ouabain and furosemide. Thus the transport mechanism has properties similar to those described for other exocrine glands. Analysis of 3H-ouabain binding sites and determination of intracellular ions by energy dispersive x-ray microanalysis indicates that the transepithelial pathway for Cl flux may be via a distinct group of cells located at the ductal pole of the acinus of two of the gland types; termed mucous and seromucous.

Experimental Investigation of Gas/Slag/Matte/Tridymite Equilibria in the Cu-Fe-O-S-Si System in Controlled Gas Atmospheres: Experimental Results at 1473 K (1200 °C) and P(SO2) = 0.25 atm

NASA Astrophysics Data System (ADS)

Fallah-Mehrjardi, Ata; Hidayat, Taufiq; Hayes, Peter C.; Jak, Evgueni

2017-12-01

Experimental studies were undertaken to determine the gas/slag/matte/tridymite equilibria in the Cu-Fe-O-S-Si system at 1473 K (1200 °C), P(SO2) = 0.25 atm, and a range of P(O2)'s. The experimental methodology involved high-temperature equilibration using a substrate support technique in controlled gas atmospheres (CO/CO2/SO2/Ar), rapid quenching of equilibrium phases, followed by direct measurement of the chemical compositions of the phases with Electron Probe X-ray Microanalysis (EPMA). The experimental data for slag and matte were presented as a function of copper concentration in matte (matte grade). The data provided are essential for the evaluation of the effect of oxygen potential under controlled atmosphere on the matte grade, liquidus composition of slag and chemically dissolved copper in slag. The new data provide important accurate and reliable quantitative foundation for improvement of the thermodynamic databases for copper-containing systems.

Characterization of Discontinuous Coarsening Reaction Products in INCONEL® Alloy 740H® Fusion Welds

NASA Astrophysics Data System (ADS)

Bechetti, Daniel H.; Dupont, John N.; Watanabe, Masashi; de Barbadillo, John J.

2017-04-01

Characterization of γ' coarsened zones (CZs) in alloy 740H fusion welds via a variety of electron microscopy techniques was conducted. The effects of solute partitioning during nonequilibrium solidification on the amount of strengthening precipitates along the grain boundaries were evaluated via electron-probe microanalysis and scanning electron microscopy. Electron backscatter diffraction was used to present evidence for the preferential growth of CZs toward regions of lower γ' content, even if growth in that direction increases grain boundary area. Scanning electron microscopy and image analysis were used to quantify the propensity for CZs to develop along certain segments of the grain boundaries, as governed by the local variations in γ' content. Scanning transmission electron microscopy with X-ray energy-dispersive spectrometry (XEDS) was used to assess the compositions of the matrix and precipitate phases within the CZs and to quantify the segregation of alloying components to the reaction front. Thermodynamic and kinetic modeling were used to compare calculated and experimental compositions. The work presented here provides new insight into the progression of the discontinuous coarsening (DC) reaction in a complex engineering alloy.

Viscosity Measurements of "FeO"-SiO2 Slag in Equilibrium with Metallic Fe

NASA Astrophysics Data System (ADS)

Chen, Mao; Raghunath, Sreekanth; Zhao, Baojun

2013-06-01

The current study delivered the measurements of viscosities in the system "FeO"-SiO2 in equilibrium with metallic Fe in the composition range between 15 and 40 wt pct SiO2. The experiments were carried out in the temperature range of 1473 K to 1773 K (1200 °C to 1500 °C) using a rotational spindle technique. An analysis of the quenched sample by electron probe X-ray microanalysis (EPMA) after the viscosity measurement enables the composition and microstructure of the slag to be directly linked with the viscosity. The current results are compared with available literature data. The significant discrepancies of the viscosity measurements in this system have been clarified. The possible reasons affecting the accuracy of the viscosity measurement have been discussed. The activation energies derived from the experimental data have a sharp increase at about 33 wt pct SiO2, which corresponds to the composition of fayalite (Fe2SiO4). The modified quasi-chemical model was constructed in the system "FeO"-SiO2 to describe the current viscosity data.

Nano-chemo-mechanical signature of conventional oil-well cement systems: Effects of elevated temperature and curing time

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

Krakowiak, Konrad J., E-mail: kjkrak@mit.edu; Thomas, Jeffrey J., E-mail: JThomas39@slb.com; Musso, Simone, E-mail: SMusso@slb.com

2015-01-15

With ever more challenging (T,p) environments for cementing applications in oil and gas wells, there is a need to identify the fundamental mechanisms of fracture resistant oil well cements. We report results from a multi-technique investigation of behavior and properties of API class G cement and silica-enriched cement systems subjected to hydrothermal curing from 30 °C to 200 °C; including electron probe microanalysis, X-ray diffraction, thermogravimetry analysis, electron microscopy, neutron scattering (SANS), and fracture scratch testing. The results provide a new insight into the link between system chemistry, micro-texture and micro-fracture toughness. We suggest that the strong correlation found betweenmore » chemically modulated specific surface and fracture resistance can explain the drop in fracture properties of neat oil-well cements at elevated temperatures; the fracture property enhancement in silica-rich cement systems, between 110° and 175 °C; and the drop in fracture properties of such systems through prolonged curing over 1 year at 200 °C.« less

Diffusion bonding of titanium to 304 stainless steel

NASA Astrophysics Data System (ADS)

Ghosh, M.; Bhanumurthy, K.; Kale, G. B.; Krishnan, J.; Chatterjee, S.

2003-11-01

Diffusion bonding between commercially pure titanium and an austenitic stainless steel (AISI 304) has been carried out in the temperature range of 850-950 °C for 2 h at uniaxial pressure of 3 MPa in vacuum. The microstructure of the diffusion zone has been analysed by optical and scanning electron microscopy (SEM). The interdiffusion of the diffusing species across the interface has been evaluated by electron probe microanalysis (EPMA). The reaction products formed at the interface have been identified by X-ray diffraction technique. It has been observed that the diffusion zone is dominated by the presence of the σ phase close to the stainless steel side and the solid solution of β-Ti (solutes are Fe, Cr and Ni) close to the titanium. The presence of Fe 2Ti and FeTi has been found in the reaction zone. It has been observed that the bond strength (˜222 MPa) is highest for the couple processed at 850 °C and this value decreases with rise in joining temperature. The variation of strength of the transition joints is co-related with the microstructural characteristics of the diffusion zone.

Projection x-ray topography system at 1-BM x-ray optics test beamline at the advanced photon source

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

Stoupin, Stanislav, E-mail: sstoupin@aps.anl.gov; Liu, Zunping; Trakhtenberg, Emil

2016-07-27

Projection X-ray topography of single crystals is a classic technique for the evaluation of intrinsic crystal quality of large crystals. In this technique a crystal sample and an area detector (e.g., X-ray film) collecting intensity of a chosen crystallographic reflection are translated simultaneously across an X-ray beam collimated in the diffraction scattering plane (e.g., [1, 2]). A bending magnet beamline of a third-generation synchrotron source delivering x-ray beam with a large horizontal divergence, and therefore, a large horizontal beam size at a crystal sample position offers an opportunity to obtain X-ray topographs of large crystalline samples (e.g., 6-inch wafers) inmore » just a few exposures. Here we report projection X-ray topography system implemented recently at 1-BM beamline of the Advanced Photon Source. A selected X-ray topograph of a 6-inch wafer of 4H-SiC illustrates capabilities and limitations of the technique.« less

Characterization of retrieved orthodontic miniscrew implants.

PubMed

Eliades, Theodore; Zinelis, Spiros; Papadopoulos, Moschos A; Eliades, George

2009-01-01

The purposes of this study were to characterize the morphologic, structural, and compositional alterations and to assess any hardness changes in used orthodontic miniscrew implants. Eleven miniscrew implants (Aarhus Anchorage System, Medicon eG, Tuttlingen, Germany) placed in 5 patients were retrieved after successful service of 3.5 to 17.5 months; none showed signs of mobility or failure. These implants, and brand-, type-, and size-matched specimens as controls, were subjected to multi-technique characterization. Optical microscopy indicated loss of gloss with variable discoloration. Scanning electron microscopy and x-ray microanalysis showed morphologic alteration of the miniscrew implant surfaces with integuments formed on the surface. The materials precipitated on the surfaces were sodium, potassium, chlorine, iron, calcium, and phosphorus from the contact of the implant with biologic fluids such as blood and exudates, forming sodium chloride, potassium chloride, and calcium-phosphorus precipitates. The composition of the implant was similar to that of a titanium alloy. X-ray microtomography analysis showed no bulk structure alterations. Vickers microhardness testing showed no increased bulk or surface hardness of the retrieved specimens compared with the controls, excluding the possibility of strain-hardening phenomena as a result of self-tapping and self-drilling placement and related loading conditions. Used titanium-alloy miniscrew implants have morphologic and surface structural alterations including adsorption of an integument that is calcified as a result of contact of the implants with biologic fluids. Randomly organized osseointegration islets on these smooth titanium-alloy miniscrew surfaces might be enhanced by the extended period of retention in alveolar bone in spite of the smooth surface and immediate loading pattern of these implants.

The Role of Materials Degradation and Analysis in the Space Shuttle Columbia Accident Investigation

NASA Technical Reports Server (NTRS)

McDanels, Steven J.

2006-01-01

The efforts following the loss of the Space Shuttle Columbia included debris recovery, reconstruction, and analysis. The debris was subjected to myriad quantitative and semiquantitative chemical analysis techniques, ranging from examination via the scanning electron microscope (SEM) with energy dispersive spectrometer (EDS) to X-Ray diffraction (XRD) and electron probe micro-analysis (EPMA). The results from the work with the debris helped the investigators determine the location where a breach likely occurred in the leading edge of the left wing during lift off of the Orbiter from the Kennedy Space Center. Likewise, the information evidenced by the debris was also crucial in ascertaining the path of impinging plasma flow once it had breached the wing. After the Columbia Accident Investigation Board (CAIB) issued its findings, the major portion of the investigation was concluded. However, additional work remained to be done on many pieces of debris from portions of the Orbiter which were not directly related to the initial impact during ascent. This subsequent work was not only performed in the laboratory, but was also performed with portable equipment, including examination via portable X-Ray fluorescence (XRF) and Fourier transform infrared spectroscopy (FTIR). Likewise, acetate and silicon-rubber replicas of various fracture surfaces were obtained for later macroscopic and fractographic examination. This paper will detail the efforts and findings from the initial investigation, as well as present results obtained by the later examination and analysis of debris from the Orbiter including its windows, bulkhead structures, and other components which had not been examined during the primary investigation.

On the clathrate form of elemental silicon, Si 136: preparation and characterisation of Na xSi 136 ( x→0)

NASA Astrophysics Data System (ADS)

Ammar, Abdelaziz; Cros, Christian; Pouchard, Michel; Jaussaud, Nicolas; Bassat, Jean-Marc; Villeneuve, Gérard; Duttine, Mathieu; Ménétrier, Michel; Reny, Edouard

2004-05-01

The clathrate form of silicon, Si 136 (otherwise known as Si 34), having a residual sodium content as low as 35 ppm (i.e., x˜0.0058 in Na xSi 136), has been prepared by thermal decomposition of NaSi under high vacuum, followed by several other treatments under vacuum, and completed by repeated reactions with iodine. The residual amount of sodium has been determined by a combination of analytic and spectroscopic methods involving XRD, electron probe microanalysis, atomic absorption, NMR and EPR. This latter technique proved to be very appropriate to the characterisation of very diluted sodium atoms in such clathrate structure and to the quantitative determination of its residual concentration.

Observation of the strain field near the Si(111) 7 x 7 surface with a new X-ray diffraction technique.

PubMed

Emoto, T; Akimoto, K; Ichimiya, A

1998-05-01

A new X-ray diffraction technique has been developed in order to measure the strain field near a solid surface under ultrahigh vacuum (UHV) conditions. The X-ray optics use an extremely asymmetric Bragg-case bulk reflection. The glancing angle of the X-rays can be set near the critical angle of total reflection by tuning the X-ray energy. Using this technique, rocking curves for Si surfaces with different surface structures, i.e. a native oxide surface, a slightly oxide surface and an Si(111) 7 x 7 surface, were measured. It was found that the widths of the rocking curves depend on the surface structures. This technique is efficient in distinguishing the strain field corresponding to each surface structure.

Influence of Cu-Ti thin film surface properties on antimicrobial activity and viability of living cells.

PubMed

Wojcieszak, Damian; Kaczmarek, Danuta; Antosiak, Aleksandra; Mazur, Michal; Rybak, Zbigniew; Rusak, Agnieszka; Osekowska, Malgorzata; Poniedzialek, Agata; Gamian, Andrzej; Szponar, Bogumila

2015-11-01

The paper describes properties of thin-film coatings based on copper and titanium. Thin films were prepared by co-sputtering of Cu and Ti targets in argon plasma. Deposited coatings consist of 90at.% of Cu and 10at.% of Ti. Characterization of the film was made on the basis of investigations of microstructure and physicochemical properties of the surface. Methods such as scanning electron microscopy, x-ray microanalysis, x-ray diffraction, x-ray photoelectron spectroscopy, atomic force microscopy, optical profilometry and wettability measurements were used to assess the properties of deposited thin films. An impact of Cu-Ti coating on the growth of selected bacteria and viability of the living cells (line L929, NCTC clone 929) was described in relation to the structure, surface state and wettability of the film. It was found that as-deposited films were amorphous. However, in such surroundings the nanocrystalline grains of 10-15nm and 25-35nm size were present. High surface active area with a roughness of 8.9nm, had an effect on receiving relatively high water contact angle value (74.1°). Such wettability may promote cell adhesion and result in an increase of the probability of copper ion transfer from the film surface into the cell. Thin films revealed bactericidal and fungicidal effects even in short term-contact. High activity of prepared films was directly related to high amount (ca. 51 %) of copper ions at 1+ state as x-ray photoelectron spectroscopy results have shown. Copyright © 2015 Elsevier B.V. All rights reserved.

Remediation of a historically Pb contaminated soil using a model natural Mn oxide waste.

PubMed

McCann, Clare M; Gray, Neil D; Tourney, Janette; Davenport, Russell J; Wade, Matthew; Finlay, Nina; Hudson-Edwards, Karen A; Johnson, Karen L

2015-11-01

A natural Mn oxide (NMO) waste was assessed as an in situ remediation amendment for Pb contaminated sites. The viability of this was investigated using a 10 month lysimeter trial, wherein a historically Pb contaminated soil was amended with a 10% by weight model NMO. The model NMO was found to have a large Pb adsorption capacity (qmax 346±14 mg g(-1)). However, due to the heterogeneous nature of the Pb contamination in the soils (3650.54-9299.79 mg kg(-1)), no treatment related difference in Pb via geochemistry could be detected. To overcome difficulties in traditional geochemical techniques due to pollutant heterogeneity we present a new method for unequivocally proving metal sorption to in situ remediation amendments. The method combines two spectroscopic techniques; namely electron probe microanalysis (EPMA) and X-ray photoelectron spectroscopy (XPS). Using this we showed Pb immobilisation on NMO, which were Pb free prior to their addition to the soils. Amendment of the soil with exogenous Mn oxide had no effect on microbial functioning, nor did it perturb the composition of the dominant phyla. We conclude that NMOs show excellent potential as remediation amendments. Copyright © 2015 The Authors. Published by Elsevier Ltd.. All rights reserved.

Imaging interactions of metal oxide nanoparticles with macrophage cells by ultra-high resolution scanning electron microscopy techniques†

PubMed Central

Plascencia-Villa, Germán; Starr, Clarise R.; Armstrong, Linda S.; Ponce, Arturo

2016-01-01

Use of engineered metal oxide nanoparticles in a plethora of biological applications and custom products has warned about some possible dose-dependent cytotoxic effects. Macrophages are key components of the innate immune system used to study possible toxic effects and internalization of different nanoparticulate materials. In this work, ultra-high resolution field emission scanning electron microscopy (FE-SEM) was used to offer new insights into the dynamical processes of interaction of nanomaterials with macrophage cells dosed with different concentrations of metal oxide nanoparticles (CeO2, TiO2 and ZnO). The versatility of FE-SEM has allowed obtaining a detailed characterization of processes of adsorption and endocytosis of nanoparticles, by using advanced analytical and imaging techniques on complete unstained uncoated cells, including secondary electron imaging, high-sensitive backscattered electron imaging, X-ray microanalysis and stereoimaging. Low voltage BF/DF-STEM confirmed nanoparticle adsorption and internalization into endosomes of CeO2 and TiO2, whereas ZnO develop apoptosis after 24 h of interaction caused by dissolution and invasion of cell nucleus. Ultra-high resolution scanning electron microscopy techniques provided new insights into interactions of inorganic nanoparticles with macrophage cells with high spatial resolution. PMID:23023106

Ethanol fixed brain imaging by phase-contrast X-ray technique

NASA Astrophysics Data System (ADS)

Takeda, Tohoru; Thet-Thet-Lwin; Kunii, Takuya; Sirai, Ryota; Ohizumi, Takahito; Maruyama, Hiroko; Hyodo, Kazuyuki; Yoneyama, Akio; Ueda, Kazuhiro

2013-03-01

The two-crystal phase-contrast X-ray imaging technique using an X-ray crystal interferometer can depict the fine structures of rat's brain such as cerebral cortex, white matter, and basal ganglia. Image quality and contrast by ethanol fixed brain showed significantly better than those by usually used formalin fixation at 35 keV X-ray energy. Image contrast of cortex by ethanol fixation was more than 3-times higher than that by formalin fixation. Thus, the technique of ethanol fixation might be better suited to image cerebral structural detail at 35 keV X-ray energy.

New consistency tests for high-accuracy measurements of X-ray mass attenuation coefficients by the X-ray extended-range technique.

PubMed

Chantler, C T; Islam, M T; Rae, N A; Tran, C Q; Glover, J L; Barnea, Z

2012-03-01

An extension of the X-ray extended-range technique is described for measuring X-ray mass attenuation coefficients by introducing absolute measurement of a number of foils - the multiple independent foil technique. Illustrating the technique with the results of measurements for gold in the 38-50 keV energy range, it is shown that its use enables selection of the most uniform and well defined of available foils, leading to more accurate measurements; it allows one to test the consistency of independently measured absolute values of the mass attenuation coefficient with those obtained by the thickness transfer method; and it tests the linearity of the response of the counter and counting chain throughout the range of X-ray intensities encountered in a given experiment. In light of the results for gold, the strategy to be ideally employed in measuring absolute X-ray mass attenuation coefficients, X-ray absorption fine structure and related quantities is discussed.

The Perils of Electron Microprobe Analysis of Apatite

NASA Astrophysics Data System (ADS)

Henderson, C. E.; Essene, E. J.; Wang, K. L.; Zhang, Y.

2010-12-01

Accurate electron microprobe analysis of apatite is problematic, especially for F and Cl, whose concentrations are essential in calculating a non-analyzable OH component. The issues include beam-induced sample damage and temporal variation of F and Cl X-rays; both effects are mainly dependent on beam current, beam spot size and apatite orientation [1]. To establish a rigorous analytical procedure, several oriented apatite samples, including the well-known Durango and Wilberforce fluorapatites, were analyzed for a large suite of elements, including oxygen. Careful X-ray spectroscopy was performed, including selection of appropriate analytical standards, background measurement positions and comparison of area peak factors. Polarized infrared spectra on oriented apatite samples were also collected for complementary information. The results show that when apatite samples are oriented with the c-axis parallel to the electron beam, there is significant nonlinear variation (an increase or decrease, depending on measurement conditions) of F and Cl X-ray intensities during analyses, and systematically higher-than-expected F apparent concentrations, despite the careful selection of electron beam conditions from a series of X-ray time scans and zero-time count rate extrapolation. On the other hand, when the electron beam is oriented perpendicular to the c-axis, with a ≤ 15 nA beam current and a ≥ 5 µm diameter defocused beam, F and Cl X-ray intensities do not vary or vary slowly and predictably with time, yielding quantitative analysis results for the Durango and Wilberforce apatites (both containing little OH) which are in good agreement with published wet chemical analyses. Furthermore, the OH and CO2 contents inferred for three other analyzed apatite samples are roughly consistent with infrared analyses. For example, for an apatite from Silver Crater Mine in Ontario, significant deficiency in the P site, as well as extra F, was inferred from microprobe analyses. Infrared spectra show a strong band of (CO3)2- for this apatite, which indicates a possible substitution of (CO3)2-(F)- for (PO4)3-. Other techniques to mitigate temporal variation of F and Cl, including alternative metal coatings, concurrent stage movement, and cryogenic sample-cooling were attempted, but did not eliminate the disparity in measured F concentrations between the two sample orientations. Thus, we believe that F measurements on F-rich apatite samples of unknown orientation are immediately suspect and should be regarded as upper limits of true F concentration. X-ray mapping, CL imaging and subsequent quantitative analyses show compositional variations in Na, S, Si, and REE in the Durango and Wilberforce fluorapatite samples used in this study. Problems of electron beam sensitivity, X-ray intensity anisotropy due to sample orientation, and compositional heterogeneity call into question their continued use as routine microanalysis reference materials. Microanalysts are encouraged to use more robust calibration standards, such as Cl-rich or other F-poor apatites for Ca, P, O and Cl, and MgF2 for F measurements. [1] Stormer, J.C., Pierson, M.L, and Tacker, R.C. (1993) Variation of F and Cl X-ray intensity due to anisotropic diffusion in apatite during electron microprobe analysis. Am. Min., 78, 641-648.

Trioctahedral micas in xenolithic ejecta from recent volcanism of the Somma-Vesuvius (Italy): Crystal chemistry and genetic inferences

NASA Astrophysics Data System (ADS)

Balassone, Giuseppina; Scordari, Fernando; Lacalamita, Maria; Schingaro, Emanuela; Mormone, Angela; Piochi, Monica; Petti, Carmela; Mondillo, Nicola

2013-02-01

This study reports the first crystal chemical database resulting from a detailed structural investigation of trioctahedral micas found in xenolithic ejecta produced during the AD 1631, 1872 and 1944 eruptions, three explosive episodes of recent volcanic period of Vesuvius volcano (Southern Italy). Three xenolith types were selected: metamorphic/metasomatic skarns, pyrometamorphic/hydrothermally altered nodules and mafic cumulates. They are related to different magma chemistry and effusive styles: from sub-plinian and most evolved (AD 1631 eruption) to violent strombolian with medium evolution degree (AD 1872 eruption) to vulcanian-effusive, least evolved (AD 1944 eruption) event, respectively. Both xenoliths and micas were investigated employing multiple techniques: the xenoliths were characterized by X-ray fluorescence, inductively-coupled plasma-mass spectrometry, optical microscopy, X-ray powder diffraction, and quantitative energy-dispersive microanalysis; the micas were studied by electron probe microanalysis and single crystal X-ray diffraction. The mica-bearing xenoliths show variable texture and mineralogical assemblage, clearly related to their different origin. Based on the major oxide chemistry, only one xenolithic sample falls in the skarn compositional field from the Somma-Vesuvius literature, some fall close to the skarns and cumulate fields, others plot close to the syenite/foidolite/essexite field. A subgroup of the selected ejecta does not fall or approach any of the compositional fields. Trace and rare earth element patterns show some petrological affinity between studied xenoliths and erupted magmas with typical Eu, Ta and Nb negative anomalies. Strongly depleted patterns were detected for the 1631 metamorphic/metasomatic skarns xenoliths. Three distinct mica groups were distinguished: 1) Mg-, Al-rich, low Ti-bearing, low to moderate F-bearing varieties (1631 xenolith), 2) Al-moderate, F- and Mg-rich, Ti-, Fe-poor varieties (1872 xenolith), and 3) Al-, Ti- and Fe-rich, F-poor phases (1944 xenolith). All the analyzed mica crystals are 1M polytypes with the expected space group C2/m. Micas from xenoliths of the 1631 Vesuvius eruption are phlogopites characterized by a combination of low extent of oxy-type and variable extent OH- → F- substitutions, as testified by the range of F concentration (from ~ 0.20 to 0.80 apfu). Micas from xenoliths of the 1872 Vesuvius eruption exhibit structural peculiarities typical of fluorophlogopites, i.e. OH- → F- substitution is predominant. Micas from the xenolith of the 1944 Vesuvius eruption display features typical of oxy-substituted micas. The variability of the crystal chemical features of the studied micas is consistent with the remarkable variation of their host rocks. Micas from 1631 nodules are related to metasomatic, skarn-type environment, deriving from the metamorphosed wall-rocks hosting the magma reservoir. The fluorophlogopites from the 1872 xenoliths testify for strongly dehydrated environmental conditions compared to those of the 1631 and 1944 hosts. Finally, magma storage condition at depth, associated to a decreasing aH2O may have promoted major oxy-type substitutions in 1944 biotites.

Report on the 18th International Conference on X-ray and Inner-Shell Processes (X99).

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

Gemmell, D. S.; Physics

2000-01-01

The 18th conference of the series served as a forum for discussing fundamental issues in the field of x-ray and inner-shell processes and their application in various disciplines of science and technology. Special emphasis was given to the opportunities offered by modern synchrotron x-ray sources. The program included plenary talks, progress reports and poster presentations relating to new developments in the field of x-ray and inner-shell processes. The range of topics included: X-ray interactions with atoms, molecules, clusters, surfaces and solids; Decay processes for inner-shell vacancies; X-ray absorption and emission spectroscopy - Photoionization processes; Phenomena associated with highly charged ionsmore » and collisions with energetic particles; Electron-spin and -momentum spectroscopy; X-ray scattering and spectroscopy in the study of magnetic systems; Applications in materials science, biology, geosciences, and other disciplines; Elastic and inelastic x-ray scattering processes in atoms and molecules; Threshold phenomena (post-collision interaction, resonant Raman processes, etc.); Nuclear absorption and scattering of x-rays; 'Fourth-generation' x-ray sources; Processes exploiting the polarization and coherence properties of x-ray beams; Developments in experimental techniques (x-ray optics, temporal techniques, detectors); Microscopy, spectromicroscopy, and various imaging techniques; Non-linear processes and x-ray lasers; Ionization and excitation induced by charged particles and by x-rays; and Exotic atoms (including 'hollow' atoms and atoms that contain 'exotic' particles).« less

Nonlinear X-Ray and Auger Spectroscopy at X-Ray Free-Electron Laser Sources

NASA Astrophysics Data System (ADS)

Rohringer, Nina

2015-05-01

X-ray free-electron lasers (XFELs) open the pathway to transfer non-linear spectroscopic techniques to the x-ray domain. A promising all x-ray pump probe technique is based on coherent stimulated electronic x-ray Raman scattering, which was recently demonstrated in atomic neon. By tuning the XFEL pulse to core-excited resonances, a few seed photons in the spectral tail of the XFEL pulse drive an avalanche of resonant inelastic x-ray scattering events, resulting in exponential amplification of the scattering signal by of 6-7 orders of magnitude. Analysis of the line profile of the emitted radiation permits to demonstrate the cross over from amplified spontaneous emission to coherent stimulated resonance scattering. In combination with statistical covariance mapping, a high-resolution spectrum of the resonant inelastic scattering process can be obtained, opening the path to coherent stimulated x-ray Raman spectroscopy. An extension of these ideas to molecules and a realistic feasibility study of stimulated electronic x-ray Raman scattering in CO will be presented. Challenges to realizing stimulated electronic x-ray Raman scattering at present-day XFEL sources will be discussed, corroborated by results of a recent experiment at the LCLS XFEL. Due to the small gain cross section in molecular targets, other nonlinear spectroscopic techniques such as nonlinear Auger spectroscopy could become a powerful alternative. Theory predictions of a novel pump probe technique based on resonant nonlinear Auger spectroscopic will be discussed and the method will be compared to stimulated x-ray Raman spectroscopy.

Quantitative Electron-Excited X-Ray Microanalysis of Borides, Carbides, Nitrides, Oxides, and Fluorides with Scanning Electron Microscopy/Silicon Drift Detector Energy-Dispersive Spectrometry (SEM/SDD-EDS) and NIST DTSA-II.

PubMed

Newbury, Dale E; Ritchie, Nicholas W M

2015-10-01

A scanning electron microscope with a silicon drift detector energy-dispersive X-ray spectrometer (SEM/SDD-EDS) was used to analyze materials containing the low atomic number elements B, C, N, O, and F achieving a high degree of accuracy. Nearly all results fell well within an uncertainty envelope of ±5% relative (where relative uncertainty (%)=[(measured-ideal)/ideal]×100%). Quantification was performed with the standards-based "k-ratio" method with matrix corrections calculated based on the Pouchou and Pichoir expression for the ionization depth distribution function, as implemented in the NIST DTSA-II EDS software platform. The analytical strategy that was followed involved collection of high count (>2.5 million counts from 100 eV to the incident beam energy) spectra measured with a conservative input count rate that restricted the deadtime to ~10% to minimize coincidence effects. Standards employed included pure elements and simple compounds. A 10 keV beam was employed to excite the K- and L-shell X-rays of intermediate and high atomic number elements with excitation energies above 3 keV, e.g., the Fe K-family, while a 5 keV beam was used for analyses of elements with excitation energies below 3 keV, e.g., the Mo L-family.

Effect of Gold on the Microstructural Evolution and Integrity of a Sintered Silver Joint

DOE PAGES

Muralidharan, Govindarajan; Leonard, Donovan N.; Meyer, Harry M.

2017-01-05

There is a need for next-generation, high-performance power electronic packages and systems employing wide band gap devices to operate at high temperatures in automotive and electric grid applications. Sintered silver joints are currently being evaluated as an alternative to Pb-free solder joints. Of particular interest is the development of joints based on silver paste consisting of nanoscale or micron scale particles that can be processed without the application of an external pressure. Microstructural evolution at the interface of a pressureless sintered silver joint formed between a SiC die with a Ti/Ni/Au metallization and an Active Metal Brazed substrate with Agmore » metallization at 250 °C was evaluated using Scanning Electron Microscopy, X-ray microanalysis, and X-ray Photo Electron Spectroscopy. Results from Focused Ion Beam cross-sections show that during sintering, the pores in the sintered region close to the Au layer tend to be smaller and are oriented predominantly with their longer dimension oriented parallel to the interface. With further densification, this results in the alignment of small pores parallel to the interface, creating a path for easy crack propagation. Lastly, X-ray microchemical analyses results confirm interdiffusion between Au and Ag and that a region with poor mechanical strength is formed at the edge of this region of interdiffusion.« less

Microbial synthesis of core/shell gold/palladium nanoparticles for applications in green chemistry

PubMed Central

Deplanche, Kevin; Merroun, Mohamed L.; Casadesus, Merixtell; Tran, Dung T.; Mikheenko, Iryna P.; Bennett, James A.; Zhu, Ju; Jones, Ian P.; Attard, Gary A.; Wood, J.; Selenska-Pobell, Sonja; Macaskie, Lynne E.

2012-01-01

We report a novel biochemical method based on the sacrificial hydrogen strategy to synthesize bimetallic gold (Au)–palladium (Pd) nanoparticles (NPs) with a core/shell configuration. The ability of Escherichia coli cells supplied with H2 as electron donor to rapidly precipitate Pd(II) ions from solution is used to promote the reduction of soluble Au(III). Pre-coating cells with Pd(0) (bioPd) dramatically accelerated Au(III) reduction, with the Au(III) reduction rate being dependent upon the initial Pd loading by mass on the cells. Following Au(III) addition, the bioPd–Au(III) mixture rapidly turned purple, indicating the formation of colloidal gold. Mapping of bio-NPs by energy dispersive X-ray microanalysis suggested Au-dense core regions and peripheral Pd but only Au was detected by X-ray diffraction (XRD) analysis. However, surface analysis of cleaned NPs by cyclic voltammetry revealed large Pd surface sites, suggesting, since XRD shows no crystalline Pd component, that layers of Pd atoms surround Au NPs. Characterization of the bimetallic particles using X-ray absorption spectroscopy confirmed the existence of Au-rich core and Pd-rich shell type bimetallic biogenic NPs. These showed comparable catalytic activity to chemical counterparts with respect to the oxidation of benzyl alcohol, in air, and at a low temperature (90°C). PMID:22399790

μX-ray fluorescence analysis of traces and calcium phosphate phases on tooth tartar interfaces using synchrotron radiation

NASA Astrophysics Data System (ADS)

Abraham, J. A.; Grenón, M. S.; Sánchez, H. J.; Valentinuzzi, M. C.; Perez, C. A.

2007-07-01

Hard dental tissues like dentine and cementum with calcified deposits (dental calculi) were studied in several human dental pieces of adult individuals from the same geographic region. A couple of cross cuts were performed at dental root level resulting in a planar slice with calculus and dental tissue exposed for analysis. The elemental content along a linear path crossing the dentine-cementum-tartar interfaces and also all over a surface was measured by X-ray fluorescence microanalysis using synchrotron radiation (μSRXRF). The concentration of elemental traces like K, V, Cu, Zn, As, Br and Sr showed different features on the analyzed regions. The possible connections with the dynamic of mineralization and biological implications are discussed. The concentrations of major elements Ca and P were also determined and the measured Ca/P molar ratio was used to estimate the average composition of calcium phosphate phases in the measured points. A deeper knowledge of the variations of the elemental compositions and the changes of the different phases will help to a better understanding of the scarcely known mechanism of calculus growing.

Conversion of Nuclear Waste to Molten Glass: Cold-Cap Reactions in Crucible Tests

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

Xu, Kai; Hrma, Pavel; Rice, Jarrett A.

2016-05-23

The feed-to-glass conversion, which comprises complex chemical reactions and phase transitions, occurs in the cold-cap zone during nuclear waste vitrification. Knowledge of the chemistry and physics of feed-to-glass conversion will help us control the conversion path by changing the melter feed makeup to maximize the glass production rate. To investigate the conversion process, we analyzed heat-treated samples of a simulated high-level waste feed using X-ray diffraction, electron probe microanalysis – wavelength dispersive X-ray spectroscopy, leaching tests, and residual anion analysis. Feed dehydration, gas evolution, and borate phase formation occurred at temperatures below 700 °C before the emerging glass-forming melt wasmore » completely connected. Above 800 °C, intermediate aluminosilicate phases and quartz particles were gradually dissolving in the continuous borosilicate melt, which expanded into transient foam. Knowledge of the chemistry and physics of feed-to-glass conversion will help us control the conversion path by changing the melter feed makeup to maximize the glass production rate.« less

Bricks in historical buildings of Toledo City: characterisation and restoration

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

Lopez-Arce, Paula; Garcia-Guinea, Javier; Gracia, Mercedes

2003-01-15

Two different types of ancient bricks (12th to 14th centuries) collected from historical buildings of Toledo (Spain) were characterised by optical microscopy, scanning electron microscopy/energy-dispersive X-ray spectrometers (SEM/EDS), electron probe microanalysis (EM), X-ray diffraction (XRD), differential thermal analysis (DTA) and {sup 57}Fe-Moessbauer spectroscopy. Physical properties such as water absorption and suction, porosity, density and compression strength were also determined. Several minerals found in the brick matrix, such as garnet, let us infer raw material sources; calcite, dolomite, illite and neoformed gehlenite and diopside phases, on temperature reached in firing; secondary calcite, on first cooling scenarios; and manganese micronodules, on latemore » pollution environments. XRD and DTA of original and refired samples supply information about firing temperatures. Additional data on firing conditions and type of the original clay are provided by the Moessbauer study. Physical properties of both types of bricks were compared and correlated with raw materials and fabric and firing technology employed. The physicochemical characterisation of these bricks provides valuable data for restoration purposes to formulate new specific bricks using neighbouring raw materials.« less

RADIOACTIVITY DOSAGE OF ORNAMENTAL GRANITIC ROCKS BASED ON CHEMICAL, MINERALOGICAL AND LITHOLOGICAL DATA

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

Salas, H.T.; Nalini, H.A. Jr.; Mendes, J.C.

2004-10-03

One hundred samples of granitic rock were collected from granite traders in Belo Horizonte. Autoradiography, optical microscopy, diffractometry, and chemical analysis (X-ray spectrometry, X-ray fluorescence, neutron activation, gravimetry and electron probe microanalysis) were used to determine the mineral assemblages and lithotypes. Autoradiographic results for several samples showed the presence of monazite, allanite and zircon. Chemical analysis revealed concentrations of uranium of {le} 30ppm, and thorium {le} 130ppm. Higher concentrations generally correlated with high concentrations of light rare earths in silica-rich rocks of granitic composition. Calculations were made of radioactive doses for floor tiles in a standard room for samples withmore » total concentration of uranium and thorium greater than 60ppm. On the basis of calculations of {sup 232}Th, {sup 40}K and {sup 226}Ra from Th, K and U analysis, the doses calculated were between 0.11 and 0.34 mSv/year, which are much lower than the acceptable international exposure standard of 1.0 mSv/year.« less

Analytical electron microscopy as a powerful tool in plant cell biology: examples using electron energy loss spectroscopy and X-ray microanalysis.

PubMed

Lichtenberger, O; Neumann, D

1997-08-01

Energy filtering transmission electron microscopy in combination with energy dispersive X-ray analysis (EDX) and quantumchemical calculations opens new possibilities for elemental and bone analysis at the ultrastructural level. The possibilities and limitations of these methods, applied to botanical samples, are discussed and some examples are given. Ca-oxalate crystals in plant cell vacuoles show a specific C K-edge in the electron energy loss spectrum (EELS), which allows a more reliable identification than light microscopical or cytochemical methods. In some dicots crystalline inclusions can be observed in different cell compartments, which are identified as silicon dioxide or calcium silicate by the fine structure of the Si L2,3-edge. Their formation is discussed on the basis of EEL-spectra and quantumchemical calculations. Examples concerning heavy metal detoxification are given for some tolerant plants. In Minuartia Zn is bound as Zn-silicate in cell walls; Armeria accumulates Cu in leaf idioblasts by chelation with phenolic compounds and Cd is precipitated as CdS/phytochelatin-complexes in tomato.

Mobility of rare earth elements in mine drainage: Influence of iron oxides, carbonates, and phosphates.

PubMed

Edahbi, Mohamed; Plante, Benoît; Benzaazoua, Mostafa; Ward, Matthew; Pelletier, Mia

2018-05-01

The geochemical behavior of rare earth elements (REE) was investigated using weathering cells. The influence of sorption and precipitation on dissolved REE mobility and fractionation is evaluated using synthetic iron-oxides, carbonates, and phosphates. Sorption cell tests are conducted on the main lithologies of the expected waste rocks from the Montviel deposit. The sorbed materials are characterized using a scanning electron microscope (SEM) equipped with a microanalysis system (energy dispersive spectroscopy EDS) (SEM-EDS), X-ray diffraction (XRD), and X-ray absorption near edge structure (XANES) in order to understand the effect of the synthetic minerals on REE mobility. The results confirm that sorption and precipitation control the mobility and fractionation of REE. The main sorbent phases are the carbonates, phosphates (present as accessory minerals in the Montviel waste rocks), and iron oxides (main secondary minerals generated upon weathering of the Montviel lithologies). The XANES results show that REE are present as trivalent species after weathering. Thermodynamic equilibrium calculations results using Visual Minteq suggest that REE could precipitate as secondary phosphates (REEPO 4 ). Copyright © 2018 Elsevier Ltd. All rights reserved.

Metallurgical characterization of experimental Ag-based soldering alloys.

PubMed

Ntasi, Argyro; Al Jabbari, Youssef S; Silikas, Nick; Al Taweel, Sara M; Zinelis, Spiros

2014-10-01

To characterize microstructure, hardness and thermal properties of experimental Ag-based soldering alloys for dental applications. Ag12Ga (AgGa) and Ag10Ga5Sn (AgGaSn) were fabricated by induction melting. Six samples were prepared for each alloy and microstructure, hardness and their melting range were determined by, scanning electron microscopy, energy dispersive X-ray (EDX) microanalysis, X-ray diffraction (XRD), Vickers hardness testing and differential scanning calorimetry (DSC). Both alloys demonstrated a gross dendritic microstructure while according to XRD results both materials consisted predominately of a Ag-rich face centered cubic phase The hardness of AgGa (61 ± 2) was statistically lower than that of AgGaSn (84 ± 2) while the alloys tested showed similar melting range of 627-762 °C for AgGa and 631-756 °C for AgGaSn. The experimental alloys tested demonstrated similar microstructures and melting ranges. Ga and Sn might be used as alternative to Cu and Zn to modify the selected properties of Ag based soldering alloys.

Metallurgical characterization of experimental Ag-based soldering alloys

PubMed Central

Ntasi, Argyro; Al Jabbari, Youssef S.; Silikas, Nick; Al Taweel, Sara M.; Zinelis, Spiros

2014-01-01

Aim To characterize microstructure, hardness and thermal properties of experimental Ag-based soldering alloys for dental applications. Materials and methods Ag12Ga (AgGa) and Ag10Ga5Sn (AgGaSn) were fabricated by induction melting. Six samples were prepared for each alloy and microstructure, hardness and their melting range were determined by, scanning electron microscopy, energy dispersive X-ray (EDX) microanalysis, X-ray diffraction (XRD), Vickers hardness testing and differential scanning calorimetry (DSC). Results Both alloys demonstrated a gross dendritic microstructure while according to XRD results both materials consisted predominately of a Ag-rich face centered cubic phase The hardness of AgGa (61 ± 2) was statistically lower than that of AgGaSn (84 ± 2) while the alloys tested showed similar melting range of 627–762 °C for AgGa and 631–756 °C for AgGaSn. Conclusion The experimental alloys tested demonstrated similar microstructures and melting ranges. Ga and Sn might be used as alternative to Cu and Zn to modify the selected properties of Ag based soldering alloys. PMID:25382945

Micro and bulk analysis of prostate tissues classified as hyperplasia

NASA Astrophysics Data System (ADS)

Kwiatek, W. M.; Banaś, A.; Banaś, K.; Cinque, G.; Dyduch, G.; Falkenberg, G.; Kisiel, A.; Marcelli, A.; Podgórczyk, M.

2007-07-01

BPH (Benign Prostatic Hyperplasia) is the most common benign neoplasm (non cancerous enlargement of the prostate gland), whose prevalence increases with age. The gland, when increased in size, exerts pressure on the urethra, causing obstruction to urine flow. The latter may result in severe urinary tract and kidney conditions. In this work prostate samples from patients diagnosed with BPH were analyzed using synchrotron radiation. Micro-analysis of the hyperplastic samples was carried out on the L-beam line at HASYLAB, DESY (Germany), while bulk analysis on selected samples was performed at the DRX2 beamline at LNF, Frascati (Italy). Microanalysis with a mono-energetic beam 15 μm in diameter confirmed that concentrations of certain elements, such as S, Mn, Cu, Fe and Zn, are good indicators of pathological disorders in prostate tissue that may be considered effective tracers of developing compliant. The concentrations of Mn, Cu, Fe and Zn are higher in hyperplastic tissues, as compared to normal ones, while for sulphur the opposite is observed. Additionally, Fe and S K-edge XANES (X-ray Absorption Near Edge Structure) spectroscopy experiments were carried out in order to determine the chemical speciation of these elements in our samples.

Backscatter X-Ray Development for Space Vehicle Thermal Protection Systems

NASA Astrophysics Data System (ADS)

Bartha, Bence B.; Hope, Dale; Vona, Paul; Born, Martin; Corak, Tony

2011-06-01

The Backscatter X-Ray (BSX) imaging technique is used for various single sided inspection purposes. Previously developed BSX techniques for spray-on-foam insulation (SOFI) have been used for detecting defects in Space Shuttle External Tank foam insulation. The developed BSX hardware and techniques are currently being enhanced to advance Non-Destructive Evaluation (NDE) methods for future space vehicle applications. Various Thermal Protection System (TPS) materials were inspected using the enhanced BSX imaging techniques, investigating the capability of the method to detect voids and other discontinuities at various locations within each material. Calibration standards were developed for the TPS materials in order to characterize and develop enhanced BSX inspection capabilities. The ability of the BSX technique to detect both manufactured and natural defects was also studied and compared to through-transmission x-ray techniques. The energy of the x-ray, source to object distance, angle of x-ray, focal spot size and x-ray detector configurations were parameters playing a significant role in the sensitivity of the BSX technique to image various materials and defects. The image processing of the results also showed significant increase in the sensitivity of the technique. The experimental results showed BSX to be a viable inspection technique for space vehicle TPS systems.

Liquid sample delivery techniques for serial femtosecond crystallography

PubMed Central

Weierstall, Uwe

2014-01-01

X-ray free-electron lasers overcome the problem of radiation damage in protein crystallography and allow structure determination from micro- and nanocrystals at room temperature. To ensure that consecutive X-ray pulses do not probe previously exposed crystals, the sample needs to be replaced with the X-ray repetition rate, which ranges from 120 Hz at warm linac-based free-electron lasers to 1 MHz at superconducting linacs. Liquid injectors are therefore an essential part of a serial femtosecond crystallography experiment at an X-ray free-electron laser. Here, we compare different techniques of injecting microcrystals in solution into the pulsed X-ray beam in vacuum. Sample waste due to mismatch of the liquid flow rate to the X-ray repetition rate can be addressed through various techniques. PMID:24914163

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

PubMed Central

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

2010-01-01

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

Single-particle investigation of summertime and wintertime Antarctic sea spray aerosols using low-Z particle EPMA, Raman microspectrometry, and ATR-FTIR imaging techniques

NASA Astrophysics Data System (ADS)

Eom, Hyo-Jin; Gupta, Dhrubajyoti; Cho, Hye-Rin; Hwang, Hee Jin; Do Hur, Soon; Gim, Yeontae; Ro, Chul-Un

2016-11-01

Two aerosol samples collected at King Sejong Korean scientific research station, Antarctica, on 9 December 2011 in the austral summer (sample S1) and 23 July 2012 in the austral winter (sample S2), when the oceanic chlorophyll a levels on the collection days of the samples were quite different, by ˜ 19 times (2.46 vs. 0.13 µg L-1, respectively), were investigated on a single-particle basis using quantitative energy-dispersive electron probe X-ray microanalysis (ED-EPMA), called low-Z particle EPMA, Raman microspectrometry (RMS), and attenuated total reflection Fourier transform infrared (ATR-FTIR) imaging techniques to obtain their characteristics based on the elemental chemical compositions, molecular species, and mixing state. X-ray analysis showed that the supermicron summertime and wintertime Antarctic aerosol samples have different elemental chemical compositions, even though all the individual particles analyzed were sea spray aerosols (SSAs); i.e., the contents of C, O, Ca, S, and Si were more elevated, whereas Cl was more depleted, for sample S1 than for sample S2. Based on qualitative analysis of the chemical species present in individual SSAs by the combined application of RMS and ATR-FTIR imaging, different organic species were observed in samples S1 and S2; i.e., Mg hydrate salts of alanine were predominant in samples S1 and S2, whereas Mg salts of fatty acids internally mixed with Mg hydrate salts of alanine were significant in sample S2. Although CaSO4 was observed significantly in both samples S1 and S2, other inorganic species, such as Na2SO4, NaNO3, Mg(NO3)2, SiO2, and CH3SO3Mg, were observed more significantly in sample S1, suggesting that those compounds may be related to the higher phytoplankton activity in summer.

Parametric studies and characterization measurements of x-ray lithography mask membranes

NASA Astrophysics Data System (ADS)

Wells, Gregory M.; Chen, Hector T. H.; Engelstad, Roxann L.; Palmer, Shane R.

1991-08-01

The techniques used in the experimental characterization of thin membranes are considered for their potential use as mask blanks for x-ray lithography. Among the parameters of interest for this evaluation are the film's stress, fracture strength, uniformity of thickness, absorption in the x-ray and visible spectral regions and the modulus and grain structure of the material. The experimental techniques used for measuring these properties are described. The accuracy and applicability of the assumptions used to derive the formulas that relate the experimental measurements to the parameters of interest are considered. Experimental results for silicon carbide and diamond films are provided. Another characteristic needed for an x-ray mask carrier is radiation stability. The number of x-ray exposures expected to be performed in the lifetime of an x-ray mask on a production line is on the order of 107. The dimensional stability requirements placed on the membranes during this period are discussed. Interferometric techniques that provide sufficient sensitivity for these stability measurements are described. A comparison is made between the different techniques that have been developed in term of the information that each technique provides, the accuracy of the various techniques, and the implementation issues that are involved with each technique.

Experimental investigation of dynamic fragmentation of laser shock-loaded by soft recovery and X-ray radiography

NASA Astrophysics Data System (ADS)

Xin, Jianting; He, Weihua; Chu, Genbai; Gu, Yuqiu

2017-06-01

Dynamic fragmentation of metal under shock pressure is an important issue for both fundamental science and practical applications. And in recent decades, laser provides a promising shock loading technique for investigating the process of dynamic fragmentation under extreme condition application of high strain rate. Our group has performed experimental investigation of dynamic fragmentation under laser shock loading by soft recovery and X-ray radiography at SGC / ó prototype laser facility. The fragments under different loading pressures were recovered by PMP foam and analyzed by X-ray micro-tomography and the improved watershed method. The experiment result showed that the bilinear exponential distribution is more appropriate for representing the fragment size distribution. We also developed X-ray radiography technique. Owing to its inherent advantage over shadowgraph technique, X-ray radiography can potentially determine quantitatively material densities by measuring the X-ray transmission. Our group investigated dynamic process of microjetting by X-ray radiography technique, the recorded radiographic images show clear microjetting from the triangular grooves in the free surface of tin sample.

Indus-2 X-ray lithography beamline for X-ray optics and material science applications

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

Dhamgaye, V. P., E-mail: vishal@rrcat.gov.in; Lodha, G. S., E-mail: vishal@rrcat.gov.in

2014-04-24

X-ray lithography is an ideal technique by which high aspect ratio and high spatial resolution micro/nano structures are fabricated using X-rays from synchrotron radiation source. The technique has been used for fabricating optics (X-ray, visible and infrared), sensors and actuators, fluidics and photonics. A beamline for X-ray lithography is operational on Indus-2. The beamline offers wide lithographic window from 1-40keV photon energy and wide beam for producing microstructures in polymers upto size ∼100mm × 100mm. X-ray exposures are possible in air, vacuum and He gas environment. The air based exposures enables the X-ray irradiation of resist for lithography and alsomore » irradiation of biological and liquid samples.« less

Multiscale tomographic analysis of heterogeneous cast Al-Si-X alloys.

PubMed

Asghar, Z; Requena, G; Sket, F

2015-07-01

The three-dimensional microstructure of cast AlSi12Ni and AlSi10Cu5Ni2 alloys is investigated by laboratory X-ray computed tomography, synchrotron X-ray computed microtomography, light optical tomography and synchrotron X-ray computed microtomography with submicrometre resolution. The results obtained with each technique are correlated with the size of the scanned volumes and resolved microstructural features. Laboratory X-ray computed tomography is sufficient to resolve highly absorbing aluminides but eutectic and primary Si remain unrevealed. Synchrotron X-ray computed microtomography at ID15/ESRF gives better spatial resolution and reveals primary Si in addition to aluminides. Synchrotron X-ray computed microtomography at ID19/ESRF reveals all the phases ≥ ∼1 μm in volumes about 80 times smaller than laboratory X-ray computed tomography. The volumes investigated by light optical tomography and submicrometre synchrotron X-ray computed microtomography are much smaller than laboratory X-ray computed tomography but both techniques provide local chemical information on the types of aluminides. The complementary techniques applied enable a full three-dimensional characterization of the microstructure of the alloys at length scales ranging over six orders of magnitude. © 2015 The Authors Journal of Microscopy © 2015 Royal Microscopical Society.

Finite Element Analysis of Surface Residual Stress in Functionally Gradient Cemented Carbide Tool

NASA Astrophysics Data System (ADS)

Su, Chuangnan; Liu, Deshun; Tang, Siwen; Li, Pengnan; Qiu, Xinyi

2018-03-01

A component distribution model is proposed for three-component functionally gradient cemented carbide (FGCC) based on electron probe microanalysis results obtained for gradient layer thickness, microstructure, and elemental distribution. The residual surface stress of FGCC-T5 tools occurring during the fabrication process is analyzed using an ANSYS-implemented finite element method (FEM) and X-ray diffraction. A comparison of the experimental and calculated values verifies the feasibility of using FEM to analyze the residual surface stress in FGCC-T5 tools. The effects of the distribution index, geometrical shape, substrate thickness, gradient layer thickness, and position of the cobalt-rich layer on residual surface stress are studied in detail.

[Contrast of Z-Pinch X-Ray Yield Measure Technique].

PubMed

Li, Mo; Wang, Liang-ping; Sheng, Liang; Lu, Yi

2015-03-01

Resistive bolometer and scintillant detection system are two mainly Z-pinch X-ray yield measure techniques which are based on different diagnostic principles. Contrasting the results from two methods can help with increasing precision of X-ray yield measurement. Experiments with different load material and shape were carried out on the "QiangGuang-I" facility. For Al wire arrays, X-ray yields measured by the two techniques were largely consistent. However, for insulating coating W wire arrays, X-ray yields taken from bolometer changed with load parameters while data from scintillant detection system hardly changed. Simulation and analysis draw conclusions as follows: (1) Scintillant detection system is much more sensitive to X-ray photons with low energy and its spectral response is wider than the resistive bolometer. Thus, results from the former method are always larger than the latter. (2) The responses of the two systems are both flat to Al plasma radiation. Thus, their results are consistent for Al wire array loads. (3) Radiation form planar W wire arrays is mainly composed of sub-keV soft X-ray. X-ray yields measured by the bolometer is supposed to be accurate because of the nickel foil can absorb almost all the soft X-ray. (4) By contrast, using planar W wire arrays, data from scintillant detection system hardly change with load parameters. A possible explanation is that while the distance between wires increases, plasma temperature at stagnation reduces and spectra moves toward the soft X-ray region. Scintillator is much more sensitive to the soft X-ray below 200 eV. Thus, although the total X-ray yield reduces with large diameter load, signal from the scintillant detection system is almost the same. (5) Both Techniques affected by electron beams produced by the loads.

Corrosion of Cu-xZn alloys in slightly alkaline chloride solutions studied by stripping voltammetry and microanalysis.

PubMed

Milosev, I; Minović, A

2001-01-01

The mechanism of corrosion of Cu-xZn alloys (x = 10-40 wt %) in slightly alkaline chloride solutions was investigated by analysing solid reaction products by energy dispersive X-ray analysis (EDS) and dissolved reaction products by differential anodic pulse stripping (DAPS) voltammetry. The corrosion process was studied under open circuit and under potentiostatic conditions at selected potentials. Pure metals were studied comparatively so that an interacting effect of particular metal components in the alloy could be determined. All four Cu-xZn alloys show an improved behaviour compared to pure metals. Under open-circuit condition both components dissolve simultaneously in the solution. With increasing immersion time the preferential, dissolution of zinc in the solution becomes pronounced. It is the highest for Cu-10Zn and the lowest for Cu-30Zn alloy. Under potentiostatic control the dissolution mechanism depends on the electrode potential and changes from exclusive dissolution of zinc to simultaneous dissolution of both components with preferential dissolution of zinc. The latter decreases, as the electrode potential becomes more positive.

Rocking-beam spectrum images and ALCHEMI of Ni{sub 50}Al{sub 40}Fe{sub 10}

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

Anderson, I.M.; Bentley, J.

1997-04-01

A rocking-beam energy-dispersive X-ray (EDX) spectrum image was acquired near the [035] zone axis of a B2-ordered alloy of composition Ni{sub 50}Al{sub 40}Fe{sub 10}. Images comparable to those acquired by Rossouw et al. were formed a posteriori by integrating the X-ray intensities in windows enclosing the Al-K, Fe-K{sub {alpha}}, and Ni-K{sub {alpha}} characteristic X-ray peaks for each pixel of the spectrum image. These images are shown along with a bright-field transmission channeling pattern (TCP), which records the signal from the bright-field STEM detector as the incident beam direction is varied with the beam-tilt coils, and an EDX spectrum from onemore » pixel of the image. The range of orientations from which the spectrum image was acquired is indicated by the square superimposed on the TCP. ALCHEMI (atom-location by channeling-enhanced microanalysis) was performed on a subset of the spectrum image using standard methods. Spectra from a series of {approximately}30 pixels along lines parallel to the (200) band were summed at each of 31 orientations relative to the band in the range 0 {le} {theta}/{theta}{sub 200} {le} 2.3. Characteristic X-ray intensities of the K-shell X-rays of Ni, Fe, and Al were extracted from the 31 summed spectra with the simplex fitting procedure of the DTSA spectral analysis software. The fraction of Fe on the `Ni`-site from this analysis, p{sub Fe`Ni`} = 23.8 {+-} 2.1%, is in excellent agreement with p{sub Fe`Ni`} = 23.7 {+-} 0.9%, which was determined by an analysis of a series of ten spectra acquired at orientations of the crystal carefully chosen so that the contributions of nonsystematic reflections are negligible.« less

New developments in high pressure x-ray spectroscopy beamline at High Pressure Collaborative Access Team

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

Xiao, Y. M., E-mail: yxiao@carnegiescience.edu; Chow, P.; Boman, G.

The 16 ID-D (Insertion Device - D station) beamline of the High Pressure Collaborative Access Team at the Advanced Photon Source is dedicated to high pressure research using X-ray spectroscopy techniques typically integrated with diamond anvil cells. The beamline provides X-rays of 4.5-37 keV, and current available techniques include X-ray emission spectroscopy, inelastic X-ray scattering, and nuclear resonant scattering. The recent developments include a canted undulator upgrade, 17-element analyzer array for inelastic X-ray scattering, and an emission spectrometer using a polycapillary half-lens. Recent development projects and future prospects are also discussed.

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

PubMed

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

2011-07-01

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

Studies of electrode structures and dynamics using coherent X-ray scattering and imaging

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

You, H.; Liu, Y.; Ulvestad, A.

2017-08-01

Electrochemical systems studied in situ with advanced surface X-ray scattering techniques are reviewed. The electrochemical systems covered include interfaces of single-crystals and nanocrystals with respect to surface modification, aqueous dissolution, surface reconstruction, and electrochemical double layers. An emphasis will be given on recent results by coherent X-ray techniques such as X-ray photon correlation spectroscopy, Bragg coherent diffraction imaging, and surface ptychography.

Development of x-ray laminography under an x-ray microscopic condition

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

Hoshino, Masato; Uesugi, Kentaro; Takeuchi, Akihisa

2011-07-15

An x-ray laminography system under an x-ray microscopic condition was developed to obtain a three-dimensional structure of laterally-extended planar objects which were difficult to observe by x-ray tomography. An x-ray laminography technique was introduced to an x-ray transmission microscope with zone plate optics. Three prototype sample holders were evaluated for x-ray imaging laminography. Layered copper grid sheets were imaged as a laminated sample. Diatomite powder on a silicon nitride membrane was measured to confirm the applicability of this method to non-planar micro-specimens placed on the membrane. The three-dimensional information of diatom shells on the membrane was obtained at a spatialmore » resolution of sub-micron. Images of biological cells on the membrane were also obtained by using a Zernike phase contrast technique.« less

Establishing nonlinearity thresholds with ultraintense X-ray pulses

NASA Astrophysics Data System (ADS)

Szlachetko, Jakub; Hoszowska, Joanna; Dousse, Jean-Claude; Nachtegaal, Maarten; Błachucki, Wojciech; Kayser, Yves; Sà, Jacinto; Messerschmidt, Marc; Boutet, Sebastien; Williams, Garth J.; David, Christian; Smolentsev, Grigory; van Bokhoven, Jeroen A.; Patterson, Bruce D.; Penfold, Thomas J.; Knopp, Gregor; Pajek, Marek; Abela, Rafael; Milne, Christopher J.

2016-09-01

X-ray techniques have evolved over decades to become highly refined tools for a broad range of investigations. Importantly, these approaches rely on X-ray measurements that depend linearly on the number of incident X-ray photons. The advent of X-ray free electron lasers (XFELs) is opening the ability to reach extremely high photon numbers within ultrashort X-ray pulse durations and is leading to a paradigm shift in our ability to explore nonlinear X-ray signals. However, the enormous increase in X-ray peak power is a double-edged sword with new and exciting methods being developed but at the same time well-established techniques proving unreliable. Consequently, accurate knowledge about the threshold for nonlinear X-ray signals is essential. Herein we report an X-ray spectroscopic study that reveals important details on the thresholds for nonlinear X-ray interactions. By varying both the incident X-ray intensity and photon energy, we establish the regimes at which the simplest nonlinear process, two-photon X-ray absorption (TPA), can be observed. From these measurements we can extract the probability of this process as a function of photon energy and confirm both the nature and sub-femtosecond lifetime of the virtual intermediate electronic state.

Development of technique for three-dimensional visualization of grain boundaries by white X-ray microbeam

NASA Astrophysics Data System (ADS)

Kajiwara, K.; Shobu, T.; Toyokawa, H.; Sato, M.

2014-04-01

A technique for three-dimensional visualization of grain boundaries was developed at BL28B2 at SPring-8. The technique uses white X-ray microbeam diffraction and a rotating slit. Three-dimensional images of small silicon single crystals filled in a plastic tube were successfully obtained using this technique for demonstration purposes. The images were consistent with those obtained by X-ray computed tomography.

Supramolecular structure of 5-aminosalycilic acid/halloysite composites.

PubMed

Viseras, Maria-Teresa; Aguzzi, Carola; Cerezo, Pilar; Cultrone, Giuseppe; Viseras, Cesar

2009-05-01

This paper assesses the supramolecular structure of nanocomposites prepared by including the anti-inflammatory drug 5-aminosalycilic acid in halloysite nanotubes. Halloysite tubes have sub-micron individual lengths with outer diameters ∼0.1 µm, as observed by FESEM. The mercury intrusion plots showed bimodal profiles with pore dimensions ∼10 and 0.06 µm. X-ray diffraction and thermogravimetric results revealed changes in the hydration form of the clay after the interaction. The groups associated to the interaction were studied by FTIR. The location of the drug in the composites was determined after uranium staining of its amino groups by X-EDS microanalysis coupled with HREM. The drug was located both inside and on the surface of the halloysite nanotubes. These results confirm the occurrence of two concomitant interaction mechanisms: rapid adsorption of 5-ASA at the external halloysite surface followed by slow adsorption of the drug inside the tubes.

Single-particle characterization of indoor aerosol particles collected at an underground shopping area in Seoul, Korea.

PubMed

Maskey, Shila; Kang, TaeHee; Jung, Hae-Jin; Ro, Chul-Un

2011-02-01

In this study, single-particle characterization of aerosol particles collected at an underground shopping area was performed for the first time. A quantitative single-particle analytical technique, low-Z particle electron probe X-ray microanalysis, was used to characterize a total of 7900 individual particles for eight sets of aerosol samples collected at an underground shopping area in Seoul, Korea. Based on secondary electron images and X-ray spectral data of individual particles, fourteen particle types were identified, in which primary soil-derived particles were the most abundant, followed by carbonaceous, Fe-containing, secondary soil-derived, and secondary sea-salt particles. Carbonaceous particles exist in three types: organic carbon, carbon-rich, and CNO-rich. A significant number of textile particles with chemical composition C, N, and O were encountered in some of the aerosol samples, which were from the textile shops and/or from clothes of passersby. Primary soil-derived particles showed seasonal variation, with peak values in spring samples, reflecting higher air exchange between indoor and outdoor environments in the spring. Secondary soil-derived, secondary sea-salt, and ammonium sulfate particles were frequently encountered in winter samples. Fe-containing particles, contributed from a nearby subway station, were in the range of about 19% relative abundances for all samples. In underground shopping areas, particulate matters can be a considerable health hazard to the workers, shoppers, passersby, and shop-keepers as they spend their considerable time in this closed microenvironment. However, no study on the characteristics of indoor aerosols in an underground shopping area has been reported to our knowledge. This work provides detailed information on characteristics of underground shopping area aerosols on a single particle level. © 2010 John Wiley & Sons A/S.

A whole-system approach to x-ray spectroscopy in cargo inspection systems

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

Langeveld, Willem G. J.; Gozani, Tsahi; Ryge, Peter

The bremsstrahlung x-ray spectrum used in high-energy, high-intensity x-ray cargo inspection systems is attenuated and modified by the materials in the cargo in a Z-dependent way. Therefore, spectroscopy of the detected x rays yields information about the Z of the x-rayed cargo material. It has previously been shown that such ZSpectroscopy (Z-SPEC) is possible under certain circumstances. A statistical approach, Z-SCAN (Z-determination by Statistical Count-rate ANalysis), has also been shown to be effective, and it can be used either by itself or in conjunction with Z-SPEC when the x-ray count rate is too high for individual x-ray spectroscopy. Both techniquesmore » require fast x-ray detectors and fast digitization electronics. It is desirable (and possible) to combine all techniques, including x-ray imaging of the cargo, in a single detector array, to reduce costs, weight, and overall complexity. In this paper, we take a whole-system approach to x-ray spectroscopy in x-ray cargo inspection systems, and show how the various parts interact with one another. Faster detectors and read-out electronics are beneficial for both techniques. A higher duty-factor x-ray source allows lower instantaneous count rates at the same overall x-ray intensity, improving the range of applicability of Z-SPEC in particular. Using an intensity-modulated advanced x-ray source (IMAXS) allows reducing the x-ray count rate for cargoes with higher transmission, and a stacked-detector approach may help material discrimination for the lowest attenuations. Image processing and segmentation allow derivation of results for entire objects, and subtraction of backgrounds. We discuss R and D performed under a number of different programs, showing progress made in each of the interacting subsystems. We discuss results of studies into faster scintillation detectors, including ZnO, BaF{sub 2} and PbWO{sub 4}, as well as suitable photo-detectors, read-out and digitization electronics. We discuss high-duty-factor linear-accelerator x-ray sources and their associated requirements, and how such sources improve spectroscopic techniques. We further discuss how image processing techniques help in correcting for backgrounds and overlapping materials. In sum, we present an integrated picture of how to optimize a cargo inspection system for x-ray spectroscopy.« less

Advances in photographic X-ray imaging for solar astronomy

NASA Technical Reports Server (NTRS)

Moses, J. Daniel; Schueller, R.; Waljeski, K.; Davis, John M.

1989-01-01

The technique of obtaining quantitative data from high resolution soft X-ray photographic images produced by grazing incidence optics was successfully developed to a high degree during the Solar Research Sounding Rocket Program and the S-054 X-Ray Spectrographic Telescope Experiment Program on Skylab. Continued use of soft X-ray photographic imaging in sounding rocket flights of the High Resolution Solar Soft X-Ray Imaging Payload has provided opportunities to further develop these techniques. The developments discussed include: (1) The calibration and use of an inexpensive, commercially available microprocessor controlled drum type film processor for photometric film development; (2) The use of Kodak Technical Pan 2415 film and Kodak SO-253 High Speed Holographic film for improved resolution; and (3) The application of a technique described by Cook, Ewing, and Sutton for determining the film characteristics curves from density histograms of the flight film. Although the superior sensitivity, noise level, and linearity of microchannel plate and CCD detectors attracts the development efforts of many groups working in soft X-ray imaging, the high spatial resolution and dynamic range as well as the reliability and ease of application of photographic media assures the continued use of these techniques in solar X-ray astronomy observations.

Structural similarities between hematoidin crystals and asteroid bodies: evidence of lipid composition.

PubMed

Brenner, D S; Drachenberg, C B; Papadimitriou, J C

2001-02-01

Hematoidin crystals (HC) are found in tissues where extravasated erythrocytes undergo degradation. Previous studies have determined that hematoidin is composed, in part, of a bilirubin-like pigment. In a previous study (Papadimitriou and Drachenberg, Ultrastruct. Pathol. 16, 413-421, 1992), we demonstrated that giant cell asteroid bodies (AB) are formed by membrane lipid bilayers. We evaluated three cases in which HC developed within splenic infarcts. The crystals were analyzed by light microscopy (LM), electron microscopy (EM), and X-ray microanalysis. A case of sarcoidosis with multiple epithelioid granulomas containing AB was studied for comparison. By LM the HC demonstrated intense, golden-color, fine threads, both intracellularly and extracellularly, in small and large clusters, and in radiating, star-shape patterns ranging in size from 2 to 200 microm. By EM the HC were composed of a core of empty clefts, consistent with dissolved lipids, suggestive of cholesterol crystals, and were surrounded by myelinoid membrane aggregates. The AB showed by LM significant morphological similarities with the intracellular HC. By EM, the AB were composed of a core of dense phospholipid bilayer tubes surrounded by a halo of myelinoid membranes. No accumulation of specific elements was found in either HC or AB by X-ray microanalysis. HC and AB show a similar star-shape morphology by both LM and EM. We postulate that this shape is due to the physicochemical properties of the accumulated lipids which originate from superfluous cell membranes created during cell fusion in the case of AB and after cellular (predominantly red cell) breakdown in the case of HC. The golden color of the HC likely results from adsorption of hydrophobic bilirubin-like pigments left over from erythrocyte breakdown into the accumulated lipids. Thus, this study shows two different (patho)physiological processes that lead to a markedly similar morphological end-product and provides further support to our proposed mechanism for AB formation.

X-ray microanalysis of rotavirus-infected mouse intestine: A new concept of diarrhoeal secretion

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

Spencer, A.J.; Osborne, M.P.; Haddon, S.J.

1990-05-01

Neonatal mice were infected at 7 days of age with rotavirus (epizootic diarrhea of infant mice (EDIM) virus) and killed at 24-h intervals postinfection (PI). Cytoplasmic concentrations of Na, Mg, P, S, Cl, K, and Ca intestinal epithelial cells from infected and age-matched control animals were measured by x-ray microanalysis. In villus tip cells, Ca concentration increased at 24-96 h PI; Na concentration increased at 24-72 h PI; Ca and Na concentrations were near normal by 168 h PI. K concentration decreased 24-72 h PI, and Cl concentration decreased 48-96 h PI. In crypt cells, changes were observed without amore » discernible pattern: at 96 h PI, Na, Mg, S, and Cl concentrations increased and K concentration decreased; at 120 h PI, the concentrations of all elements except Na and Ca increased. In villus base cells, the mean concentrations of all elements except Ca peaked at 48-72 h PI and at 120 h PI. Na and Cl concentrations increased dramatically in some cells from 48 h PI onward. All the above concentration values were obtained from freeze-dried specimens and expressed in millimoles per kilogram of dry weight. Conversion of a limited number of data, pertaining to villus base cells, from dry weight to wet weight was possible. This conversion revealed that villus base cells in infected animals were more hydrated than corresponding cells from control animals. Also, the Na and Cl concentrations in mmol/kg H2O were significantly higher in villus base cells from infected animals than in those from corresponding controls: 137 +/- 7 versus 38 +/- 4 (Na) and 121 +/- 5 versus 89 +/- 6 (Cl). Wet weight concentrations of other elements were either the same (Mg) or lower (P, S, and K) after infection with virus.« less

The lack of age-pigments and the alterations in intracellular monovalent electrolytes in spontaneously hypertensive, stroke-prone (SHRsp) rats as revealed by electron microscopy and X-ray microanalysis

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

Zs.-Nagy, I.; Zs.-Nagy, V.; Casoli, T.

1989-01-01

Male, spontaneously hypertensive, stroke-prone (SHRsp) rats established by Okamoto et al. were studied. About 80% of the males of this strain have a particularly short life span (33-41 weeks); they display a considerable hypertension (above 220 mmHg) and a tendency for plurifocal brain strokes. Hypertension and strokes can be provoked in an accelerated and synchronized fashion by supplementing 1% NaCl into their drinking water. Symptoms of the appearance of brain strokes can be judged from characteristic signs of motor disorders, and can be established also by pathohistology. Since hypertension and arteriosclerosis are frequently involved in aging, the question we intendedmore » to answer was whether these animals may represent a model of the normal aging process or not. Two approaches are described: (1) Accumulation of lipofuscin granules in their brain, liver and myocardium was followed by transmission electron microscopy before and after the appearance of strokes. It has been established that these tissues do not show any typical accumulation of lipofuscin granules, although submicroscopic signs of an enhanced damage of cell organelles (especially of mitochondria in liver and brain cells, but not in myocardium) were encountered. (2) The intracellular monovalent composition in the brain and liver was measured by using bulk-specimen X-ray microanalysis. The intracellular Na-content (mEq/kg water) was significantly higher (170-200%) in both the brain and liver cells, whereas the K-content increased only moderately (118-130%). The results suggest that although the SHRsp rats do not represent a direct model for the normal aging process from the point of view of lipofuscin accumulation, the shifts of the monovalent electrolyte contents in the brain and liver cells observed already in the youngest ages, are similar to those observed in aged normal rats.« less

Temporal cross-correlation of x-ray free electron and optical lasers using soft x-ray pulse induced transient reflectivity.

PubMed

Krupin, O; Trigo, M; Schlotter, W F; Beye, M; Sorgenfrei, F; Turner, J J; Reis, D A; Gerken, N; Lee, S; Lee, W S; Hays, G; Acremann, Y; Abbey, B; Coffee, R; Messerschmidt, M; Hau-Riege, S P; Lapertot, G; Lüning, J; Heimann, P; Soufli, R; Fernández-Perea, M; Rowen, M; Holmes, M; Molodtsov, S L; Föhlisch, A; Wurth, W

2012-05-07

The recent development of x-ray free electron lasers providing coherent, femtosecond-long pulses of high brilliance and variable energy opens new areas of scientific research in a variety of disciplines such as physics, chemistry, and biology. Pump-probe experimental techniques which observe the temporal evolution of systems after optical or x-ray pulse excitation are one of the main experimental schemes currently in use for ultrafast studies. The key challenge in these experiments is to reliably achieve temporal and spatial overlap of the x-ray and optical pulses. Here we present measurements of the x-ray pulse induced transient change of optical reflectivity from a variety of materials covering the soft x-ray photon energy range from 500eV to 2000eV and outline the use of this technique to establish and characterize temporal synchronization of the optical-laser and FEL x-ray pulses.

Coherent x-ray diffraction imaging with nanofocused illumination.

PubMed

Schroer, C G; Boye, P; Feldkamp, J M; Patommel, J; Schropp, A; Schwab, A; Stephan, S; Burghammer, M; Schöder, S; Riekel, C

2008-08-29

Coherent x-ray diffraction imaging is an x-ray microscopy technique with the potential of reaching spatial resolutions well beyond the diffraction limits of x-ray microscopes based on optics. However, the available coherent dose at modern x-ray sources is limited, setting practical bounds on the spatial resolution of the technique. By focusing the available coherent flux onto the sample, the spatial resolution can be improved for radiation-hard specimens. A small gold particle (size <100 nm) was illuminated with a hard x-ray nanobeam (E=15.25 keV, beam dimensions approximately 100 x 100 nm2) and is reconstructed from its coherent diffraction pattern. A resolution of about 5 nm is achieved in 600 s exposure time.

Advances in X-ray Mapping for Characterization of Microstructures: Silicon Drift Detectors, Microcalorimeters, X-ray Spectrum Imaging, and Data Mining

NASA Astrophysics Data System (ADS)

Newbury, D. E.

2006-05-01

X-ray mapping, performed with the electron probe microanalyzer (EPMA) or scanning electron microscope/energy dispersive x-ray spectrometer (SEM/EDS), is one of the most popular modes of studying chemically heterogeneous microstructures [1]. Despite the maturity of the technique, now in its 50th anniversary year [2], recent remarkable advances in instrumentation and software will provide microanalysts with an even more effective and efficient microstructural characterization tool: (1) Increased x-ray mapping speed: The silicon drift detector (SDD) [3] is a new form of the familiar silicon EDS that uses the same detection physics but with a radically different design that outperforms the classic Si-EDS in nearly every way [4]: (1) the SDD operates requires only Peltier cooling to -20 oC to - 50 oC; (2) for a given detector active area, the SDD has superior resolution; (3) the SDD achieves the same resolution but with a peaking time that is 5 to 8 times faster; and (4) maximum output count rate (OCR) ranges from about 14 kHz at optimum resolution (134 eV at MnKa for a 50 mm2 area) to 500 kHz (217 eV). This OCR performance enables rapid x-ray mapping collection in the x-ray spectrum image (XSI) mode, in which a complete EDS spectrum (2048 10eV-channels) is captured at each pixel (e.g., 10 ms dwell with 1.3 ms overhead per pixel, or 185 seconds for a 128x128 pixel map). XSI collection captures all possible spectral information within the limits imposed by the spectrometer and the primary beam dose. (2) EDS with WDS resolution: The microcalorimeter EDS measures the temperature rise when a single x-ray photon is absorbed in a metal target [5]. Demonstrated resolution is 4.5 eV at Mn Ka for a broad energy range (0.2 - 10 keV) spectrometer and 2 eV (AlKa) for a low photon energy range (0.2 - 2.0 keV) version. The low energy spectrometer is sensitive to peak shape and position changes associated with chemical bonding, opening the possibility of EDS chemical-state mapping. (3) Data mining: In the XSI mode, data is captured at the rate of 100 Mbytes per XSI database or more. Efficient software tools have been developed that enable the analyst to quickly recognize major and minor constituent features in this datacube, and even to detect rare unexpected features that occur at only one pixel in a large map [6]. Advanced image cube data reduction can be achieved with tools based on statistical methods, such as principal component analysis, that quickly establishes correlations between different elements, such as distinct phases [7]. 1. Goldstein, J., Newbury, D., Joy, D., Lyman, C., Echlin, P., Lifshin, E., Sawyer, L., and Michael, J., Scanning Electron Microscopy and X-ray Microanalysis, 3rd edition (Kluwer Academic Plenum Press, New York, 2003). 2. Cosslett, E. and P. Duncumb, Nature, 177 (1956) 1172. 3. Struder, L., Fiorini, C., Gatti, E., Hartmann, R., Holl, P., Krause, N., Lechner, P., Longoni, A., Lutz, G., Kemmer, J., Meidinger, N., Popp, M., Soltau, H., and van Zanthier, C., High resolution non dispersive x-ray spectroscopy with state of the art silicon detectors, Mikrochim. Acta, Suppl, 15 (1998) 11 4. Newbury, D. SCANNING, 27 (2005) 227. 5. Wollman, D., Irwin, K., Hilton, G., Dulcie, L., Newbury, D., and Martinis, J., J. Micros. 188 (1997) 196. 6. Newbury, D. and Bright, D., SCANNING, 27 (2005) 15. 7. Kotula, P. Keenan, M., and Michael J., Micros. Microanal. 9 (2003) 1

A novel x-ray imaging system and its imaging performance

NASA Astrophysics Data System (ADS)

Yu, Chunyu; Chang, Benkang; Wang, Shiyun; Zhang, Junju; Yao, Xiao

2006-09-01

Since x-ray was discovered and applied to the imaging technology, the x-ray imaging techniques have experienced several improvements, from film-screen, x-ray image intensifier, CR to DR. To store and transmit the image information conveniently, the digital imaging is necessary for the imaging techniques in medicine and biology. Usually as the intensifying screen technique as for concerned, to get the digital image signals, the CCD was lens coupled directly to the screen, but which suffers from a loss of x-ray signal and resulted in the poor x-ray image perfonnance. Therefore, to improve the image performance, we joined the brightness intensifier, which, was named the Low Light Level (LLL) image intensifier in military affairs, between the intensifying screen and the CCD and designed the novel x-ray imaging system. This design method improved the image performance of the whole system thus decreased the x-ray dose. Comparison between two systems with and without the brightness intensifier was given in detail in this paper. Moreover, the main noise source of the image produced by the novel system was analyzed, and in this paper, the original images produced by the novel x-ray imaging system and the processed images were given respectively. It was clear that the image performance was satisfied and the x-ray imaging system can be used in security checking and many other nondestructive checking fields.

In-situ X-ray diffraction system using sources and detectors at fixed angular positions

DOEpatents

Gibson, David M [Voorheesville, NY; Gibson, Walter M [Voorheesville, NY; Huang, Huapeng [Latham, NY

2007-06-26

An x-ray diffraction technique for measuring a known characteristic of a sample of a material in an in-situ state. The technique includes using an x-ray source for emitting substantially divergent x-ray radiation--with a collimating optic disposed with respect to the fixed source for producing a substantially parallel beam of x-ray radiation by receiving and redirecting the divergent paths of the divergent x-ray radiation. A first x-ray detector collects radiation diffracted from the sample; wherein the source and detector are fixed, during operation thereof, in position relative to each other and in at least one dimension relative to the sample according to a-priori knowledge about the known characteristic of the sample. A second x-ray detector may be fixed relative to the first x-ray detector according to the a-priori knowledge about the known characteristic of the sample, especially in a phase monitoring embodiment of the present invention.

X-Ray Sum Frequency Diffraction for Direct Imaging of Ultrafast Electron Dynamics

NASA Astrophysics Data System (ADS)

Rouxel, Jérémy R.; Kowalewski, Markus; Bennett, Kochise; Mukamel, Shaul

2018-06-01

X-ray diffraction from molecules in the ground state produces an image of their charge density, and time-resolved x-ray diffraction can thus monitor the motion of the nuclei. However, the density change of excited valence electrons upon optical excitation can barely be monitored with regular diffraction techniques due to the overwhelming background contribution of the core electrons. We present a nonlinear x-ray technique made possible by novel free electron laser sources, which provides a spatial electron density image of valence electron excitations. The technique, sum frequency generation carried out with a visible pump and a broadband x-ray diffraction pulse, yields snapshots of the transition charge densities, which represent the electron density variations upon optical excitation. The technique is illustrated by ab initio simulations of transition charge density imaging for the optically induced electronic dynamics in a donor or acceptor substituted stilbene.

Pigmenting agents in Martian soils: inferences from spectral, Mossbauer, and magnetic properties of nanophase and other iron oxides in Hawaiian palagonitic soil PN-9

NASA Technical Reports Server (NTRS)

Morris, R. V.; Golden, D. C.; Lauer, H. V. Jr; Adams, J. B.

1993-01-01

We have examined a Hawaiian palagonitic tephra sample (PN-9) that has spectroscopic similarities to Martian bright regions using a number of analytical techniques, including Mossbauer and reflectance spectroscopy, X-ray diffraction, instrumental neutron activation analysis, electron probe microanalysis, transmission electron microscopy, and dithionite-citrate-bicarbonate extraction. Chemically, PN-9 has a Hawaiitic composition with alkali (and presumably silica) loss resulting from leaching by meteoric water during palagonitization; no Ce anomaly is present in the REE pattern. Mineralogically, our results show that nanophase ferric oxide (np-Ox) particles (either nanophase hematite (np-Hm) or a mixture of ferrihydrite and np-Hm) are responsible for the distinctive ferric doublet and visible-wavelength ferric absorption edge observed in Mossbauer and reflectivity spectra, respectively, for this and other spectrally similar palagonitic samples. The np-Ox particles appear to be imbedded in a hydrated aluminosilicate matrix material; no evidence was found for phyllosilicates. Other iron-bearing phases observed are titanomagnetite, which accounts for the magnetic nature of the sample; olivine; pyroxene; and glass. By analogy, np-Ox is likely the primary pigmenting agent of the bright soils and dust of Mars.

Structural, morphological and interfacial characterization of Al-Mg/TiC composites

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

Contreras, A.; Angeles-Chavez, C.; Flores, O.

2007-08-15

Morphological and structural characterization of Al-Mg/TiC composites obtained by infiltration process and wetting by the sessile drop technique were studied. Focusing at the interface, wetting of TiC substrates by molten Al-Mg-alloys at 900 deg. C was investigated. Electron probe microanalysis (EPMA) indicated that aluminum carbide (Al{sub 4}C{sub 3}) is formed at the interface and traces of TiAl{sub 3} in the wetting assemblies were detected. Scanning Electron Microscopy (SEM) observations show that TiC particles do not appear to be uniformly attacked to produce a continuous layer of Al{sub 4}C{sub 3} at the interface. Molten Al-Mg-alloys were infiltrated into TiC preforms withmore » flowing argon at a temperature of 900 deg. C. In the composites no reaction phase was observed by SEM. Quantification of the Al phase in the composite was carried out by X-ray diffraction (XRD) and Rietveld analysis. Chemical mapping analyzed by SEM shows that the Al-Mg alloy surrounds TiC particles. In the composites with 20 wt.% of Mg the Al-Mg-{beta} phase was detected through XRD.« less

Phase Equilibria of ``Cu2O''-``FeO''-CaO-MgO-Al2O3 Slags at PO2 of 10-8.5 atm in Equilibrium with Metallic Copper for a Copper Slag Cleaning Production

NASA Astrophysics Data System (ADS)

Henao, Hector M.; Pizarro, Claudio; Font, Jonkion; Moyano, Alex; Hayes, Peter C.; Jak, Evgueni

2010-12-01

Limited data are available on phase equilibria of the multicomponent slag system at the oxygen partial pressures used in the copper smelting, converting, and slag-cleaning processes. Recently, experimental procedures have been developed and have been applied successfully to characterize several complex industrial slags. The experimental procedures involve high-temperature equilibration on a substrate and quenching followed by electron probe X-ray microanalysis. This technique has been used to construct the liquidus for the “Cu2O”-“FeO”-SiO2-based slags with 2 wt pct of CaO, 0.5 wt pct of MgO, and 4.0 wt pct of Al2O3 at controlled oxygen partial pressures in equilibrium with metallic copper. The selected ranges of compositions and temperatures are directly relevant to the copper slag-cleaning processes. The new experimental equilibrium results are presented in the form of ternary sections and as a liquidus temperature vs Fe/SiO2 weight ratio diagram. The experimental results are compared with the FactSage thermodynamic model calculations.

Electrochemical Characteristics of a Diamond-Like-Carbon-Coated LiV3O8 Cathode When Used in a Li-Metal Battery with a Li-Powder Anode

NASA Astrophysics Data System (ADS)

Lee, Jae Ha; Lee, Jun Kyu; Yoon, Woo Young

2013-10-01

A diamond-like-carbon (DLC)-coated LiV3O8 cathode was synthesized for use in a rechargeable 2032-coin-type cell with a Li-powder electrode (LPE) as the anode. The LPE anode was produced using the droplet emulsion technique and was compacted by pressing. The initial discharge capacity of the LPE/DLC-coated LiV3O8 (LVO) cell was 238 mAh g-1 at a C-rate of 0.5, while that of a LPE/bare-LVO cell was 236 mAh g-1. After 50 cycles, the capacity retention rate of the DLC-coated-electrode-containing cell (92%) was higher than that of the uncoated-electrode-containing cell (77%). Results of electron probe microanalysis and Raman spectroscopy confirmed that the electrode had been coated with DLC. Scanning electron microscopy and energy dispersive X-ray spectroscopy were used to determine the sequence of formation of byproducts on the electrode after charging/discharging and to determine its surface composition. The voltage profile and impedance of the DLC-coated-electrode-containing cell were analyzed to determine the electrochemical characteristics of the DLC-coated cathode.

Experimental Phase Equilibria Studies of the Pb-Fe-O System in Air, in Equilibrium with Metallic Lead and at Intermediate Oxygen Potentials

NASA Astrophysics Data System (ADS)

Shevchenko, M.; Jak, E.

2017-12-01

The phase equilibria information on the Pb-Fe-O system is of practical importance for the improvement of the existing thermodynamic database of lead-containing slag systems (Pb-Zn-Fe-Cu-Si-Ca-Al-Mg-O). Phase equilibria of the Pb-Fe-O system have been investigated: (a) in air at temperatures between 1053 K and 1373 K (780 °C and 1100 °C); (b) in equilibrium with metallic lead at temperatures between 1053 K and 1373 K (780 °C and 1100 °C); and (c) at intermediate oxidation conditions for the liquid slag in equilibrium with two solids (spinel + magnetoplumbite), at temperatures between 1093 K and 1373 K (820 °C and 1100 °C). The high-temperature equilibration/quenching/electron probe X-ray microanalysis technique has been used to accurately determine the compositions of the phases in equilibrium in the system. The Pb and Fe concentrations in the phases were determined directly; preliminary thermodynamic modeling with FactSage was used to estimate the ferrous-to-ferric ratios and to present the results in the ternary diagram.

Ultrastructural characterization of melanosomes of the human pathogenic fungus Fonsecaea pedrosoi.

PubMed

Franzen, Anderson J; Cunha, Marcel M L; Miranda, Kildare; Hentschel, Joachim; Plattner, Helmut; da Silva, Moises B; Salgado, Claudio G; de Souza, Wanderley; Rozental, Sonia

2008-04-01

Melanin is a complex polymer widely distributed in nature and has been described as an important virulence factor in pathogenic fungi. In the majority of fungi, the mechanism of melanin formation remains unclear. In Fonsecaea pedrosoi, the major etiologic agent of chromoblastomycosis, melanin is stored in intracellular vesicles, named melanosomes. This paper details the ultrastructural aspects of melanin formation, its storage and transportation to the cell wall in the human pathogenic fungus F. pedrosoi. In this fungus, melanin synthesis within melanosomes also begins with a fibrillar matrix formation, displaying morphological and structural features similar to melanosomes from amphibian and mammalian cells. Silver precipitation based on Fontana-Masson technique for melanin detection and immunocytochemistry showed that melanosome fuses with fungal cell membrane where the melanin is released and reaches the cell wall. Melanin deposition in the fungal cell wall occurs in concentric layers. Antibodies raised against F. pedrosoi melanin revealed the sites of melanin production and storage in the melanosomes. In addition, a preliminary description of the elemental composition of this organelle by X-ray microanalysis and elemental mapping revealed the presence of calcium, phosphorus and iron concentrated in its matrix, suggesting a new functional role for these organelles as iron storage compartments.

X-ray micro-beam techniques and phase contrast tomography applied to biomaterials

NASA Astrophysics Data System (ADS)

Fratini, Michela; Campi, Gaetano; Bukreeva, Inna; Pelliccia, Daniele; Burghammer, Manfred; Tromba, Giuliana; Cancedda, Ranieri; Mastrogiacomo, Maddalena; Cedola, Alessia

2015-12-01

A deeper comprehension of the biomineralization (BM) process is at the basis of tissue engineering and regenerative medicine developments. Several in-vivo and in-vitro studies were dedicated to this purpose via the application of 2D and 3D diagnostic techniques. Here, we develop a new methodology, based on different complementary experimental techniques (X-ray phase contrast tomography, micro-X-ray diffraction and micro-X-ray fluorescence scanning technique) coupled to new analytical tools. A qualitative and quantitative structural investigation, from the atomic to the micrometric length scale, is obtained for engineered bone tissues. The high spatial resolution achieved by X-ray scanning techniques allows us to monitor the bone formation at the first-formed mineral deposit at the organic-mineral interface within a porous scaffold. This work aims at providing a full comprehension of the morphology and functionality of the biomineralization process, which is of key importance for developing new drugs for preventing and healing bone diseases and for the development of bio-inspired materials.

Diagnosis of electrocution: The application of scanning electron microscope and energy-dispersive X-ray spectroscopy in five cases.

PubMed

Visonà, S D; Chen, Y; Bernardi, P; Andrello, L; Osculati, A

2018-03-01

Deaths from electricity, generally, do not have specific findings at the autopsy. The diagnosis is commonly based on the circumstances of the death and the morphologic findings, above all the current mark. Yet, the skin injury due to an electrocution and other kinds of thermal injuries often cannot be differentiated with certainty. Therefore, there is a great interest in finding specific markers of electrocution. The search for the metallization of the skin through Scanning Electron Microscope equipped with Energy Dispersive X-Ray Spectroscopy (EDS) probe is of special importance in order to achieve a definite diagnosis in case of suspected electrocution. We selected five cases in which the electrocution was extremely likely considering the circumstances of the death. In each case a forensic autopsy was performed. Then, the skin specimens were stained with Hematoxylin Eosin and Perls. On the other hand, the skin lesions were examined with a scanning electron microscope equipped with EDS probe in order to evaluate the morphological ultrastructural features and the presence of deposits on the surface of the skin. The typical skin injury of the electrocution (current mark) were macroscopically detected in all of the cases. The microscopic examination of the skin lesions revealed the typical spherical vacuoles in the horny layer and, in the epidermis, the elongation of the cell nuclei as well as necrosis. Perls staining was negative in 4 out 6 cases. Ultrastructural morphology revealed the evident vacuolization of the horny layer, elongation of epidermic cells, coagulation of the elastic fibers. In the specimens collected from the site of contact with the conductor of case 1 and 2, the presence of the Kα peaks of iron was detected. In the corresponding specimens taken from cases 2, 4, 5 the microanalysis showed the Kα peaks of titanium. In case 3, titanium and carbon were found. In the suspicion of electrocution, the integrated use of different tools is recommended, including macroscopic observation, H&E staining, iron-specific staining, scanning electron microscopy and EDS microanalysis. Only the careful interpretation of the results provided by all these methods can allow the pathologist to correctly identify the cause of the death. Particularly, the present study suggests that the microanalysis (SEM-EDS) represents a very useful tool for the diagnosis of electrocution, allowing the detection and the identification of the metals embedded in the skin and their evaluation in the context of the ultrastructural morphology. Copyright © 2018. Published by Elsevier B.V.

Establishing nonlinearity thresholds with ultraintense X-ray pulses

DOE PAGES

Szlachetko, Jakub; Hoszowska, Joanna; Dousse, Jean-Claude; ...

2016-09-13

X-ray techniques have evolved over decades to become highly refined tools for a broad range of investigations. Importantly, these approaches rely on X-ray measurements that depend linearly on the number of incident X-ray photons. The advent of X-ray free electron lasers (XFELs) is opening the ability to reach extremely high photon numbers within ultrashort X-ray pulse durations and is leading to a paradigm shift in our ability to explore nonlinear X-ray signals. However, the enormous increase in X-ray peak power is a double-edged sword with new and exciting methods being developed but at the same time well-established techniques proving unreliable.more » Consequently, accurate knowledge about the threshold for nonlinear X-ray signals is essential. Here in this paper we report an X-ray spectroscopic study that reveals important details on the thresholds for nonlinear X-ray interactions. By varying both the incident X-ray intensity and photon energy, we establish the regimes at which the simplest nonlinear process, two-photon X-ray absorption (TPA), can be observed. From these measurements we can extract the probability of this process as a function of photon energy and confirm both the nature and sub-femtosecond lifetime of the virtual intermediate electronic state.« less

Evaluation of enamel by scanning electron microscopy green LED associated to hydrogen peroxide 35% for dental bleaching

NASA Astrophysics Data System (ADS)

Monteiro, Juliana S. C.; de Oliveira, Susana C. P. S.; Zanin, Fátima A. A.; Santos, Gustavo M. P.; Sampaio, Fernando J. P.; Gomes Júnior, Rafael Araújo; Gesteira, Maria F. M.; Vannier-Santos, Marcos A.; Pinheiro, Antônio Luiz B.

2014-02-01

Dental bleaching is a frequently requested procedure in clinical dental practice. The literature is contradictory regarding the effects of bleaching agents on both morphology and demineralization of enamel after bleaching. The aim of this study was to analyze by SEM the effect of 35% neutral hydrogen peroxide cured by green LED. Buccal surfaces of 15 pre-molars were sectioned and marked with a central groove to allow experimental and control groups on the same specimen. For SEM, 75 electron micrographs were evaluated by tree observers at 43X, 220X and 1000X. Quantitative analysis for the determination of the surface elemental composition of the samples through X-ray microanalysis by SEM was also performed. The protocol tested neither showed significant changes in mineral composition of the samples nor to dental enamel structure when compared to controls. SEM analysis allowed inferring that there were marked morphological differences between the enamel samples highlighting the need for the use of the same tooth in comparative morphological studies. The tested protocol did not cause morphological damage the enamel surface when compared to their respective controls.

Soft X-ray spectroscopy of nanoparticles by velocity map imaging

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

Kostko, O.; Xu, B.; Jacobs, M. I.

Velocity map imaging (VMI), a technique traditionally used to study chemical dynamics in the gas phase, is applied to study X-ray photoemission from aerosol nanoparticles. Soft X-rays from the Advanced Light Source synchrotron, probe a beam of nanoparticles, and the resulting photoelectrons are velocity mapped to obtain their kinetic energy distributions. A new design of the VMI spectrometer is described. The spectrometer is benchmarked by measuring vacuum ultraviolet photoemission from gas phase xenon and squalene nanoparticles followed by measurements using soft X-rays. It is demonstrated that the photoelectron distribution from X-ray irradiated squalene nanoparticles is dominated by secondary electrons. Bymore » scanning the photon energies and measuring the intensities of these secondary electrons, a near edge X-ray absorption fine structure (NEXAFS) spectrum is obtained. The NEXAFS technique is used to obtain spectra of aqueous nanoparticles at the oxygen K edge. By varying the position of the aqueous nanoparticle beam relative to the incident X-ray beam, evidence is presented such that the VMI technique allows for NEXAFS spectroscopy of water in different physical states. Finally, we discuss the possibility of applying VMI methods to probe liquids and solids via X-ray spectroscopy.« less

Soft X-ray spectroscopy of nanoparticles by velocity map imaging

DOE PAGES

Kostko, O.; Xu, B.; Jacobs, M. I.; ...

2017-05-05

Velocity map imaging (VMI), a technique traditionally used to study chemical dynamics in the gas phase, is applied to study X-ray photoemission from aerosol nanoparticles. Soft X-rays from the Advanced Light Source synchrotron, probe a beam of nanoparticles, and the resulting photoelectrons are velocity mapped to obtain their kinetic energy distributions. A new design of the VMI spectrometer is described. The spectrometer is benchmarked by measuring vacuum ultraviolet photoemission from gas phase xenon and squalene nanoparticles followed by measurements using soft X-rays. It is demonstrated that the photoelectron distribution from X-ray irradiated squalene nanoparticles is dominated by secondary electrons. Bymore » scanning the photon energies and measuring the intensities of these secondary electrons, a near edge X-ray absorption fine structure (NEXAFS) spectrum is obtained. The NEXAFS technique is used to obtain spectra of aqueous nanoparticles at the oxygen K edge. By varying the position of the aqueous nanoparticle beam relative to the incident X-ray beam, evidence is presented such that the VMI technique allows for NEXAFS spectroscopy of water in different physical states. Finally, we discuss the possibility of applying VMI methods to probe liquids and solids via X-ray spectroscopy.« less

[Development of the automatic dental X-ray film processor].

PubMed

Bai, J; Chen, H

1999-07-01

This paper introduces a multiple-point detecting technique of the density of dental X-ray films. With the infrared ray multiple-point detecting technique, a single-chip microcomputer control system is used to analyze the effectiveness of the film-developing in real time in order to achieve a good image. Based on the new technology, We designed the intelligent automatic dental X-ray film processing.

Probing Individual Ice Nucleation Events with Environmental Scanning Electron Microscopy

NASA Astrophysics Data System (ADS)

Wang, Bingbing; China, Swarup; Knopf, Daniel; Gilles, Mary; Laskin, Alexander

2016-04-01

Heterogeneous ice nucleation is one of the processes of critical relevance to a range of topics in the fundamental and the applied science and technologies. Heterogeneous ice nucleation initiated by particles proceeds where microscopic properties of particle surfaces essentially control nucleation mechanisms. Ice nucleation in the atmosphere on particles governs the formation of ice and mixed phase clouds, which in turn influence the Earth's radiative budget and climate. Heterogeneous ice nucleation is still insufficiently understood and poses significant challenges in predictive understanding of climate change. We present a novel microscopy platform allowing observation of individual ice nucleation events at temperature range of 193-273 K and relative humidity relevant for ice formation in the atmospheric clouds. The approach utilizes a home built novel ice nucleation cell interfaced with Environmental Scanning Electron Microscope (IN-ESEM system). The IN-ESEM system is applied for direct observation of individual ice formation events, determining ice nucleation mechanisms, freezing temperatures, and relative humidity onsets. Reported microanalysis of the ice nucleating particles (INP) include elemental composition detected by the energy dispersed analysis of X-rays (EDX), and advanced speciation of the organic content in particles using scanning transmission x-ray microscopy with near edge X-ray absorption fine structure spectroscopy (STXM/NEXAFS). The performance of the IN-ESEM system is validated through a set of experiments with kaolinite particles with known ice nucleation propensity. We demonstrate an application of the IN-ESEM system to identify and characterize individual INP within a complex mixture of ambient particles.

Microscopy and microanalysis of complex nanosized strengthening precipitates in new generation commercial Al-Cu-Li alloys.

PubMed

Guinel, M J-F; Brodusch, N; Sha, G; Shandiz, M A; Demers, H; Trudeau, M; Ringer, S P; Gauvin, R

2014-09-01

Precipitates (ppts) in new generation aluminum-lithium alloys (AA2099 and AA2199) were characterised using scanning and transmission electron microscopy and atom probe tomography. Results obtained on the following ppts are reported: Guinier-Preston zones, T1 (Al2 CuLi), β' (Al3 Zr) and δ' (Al3 Li). The focus was placed on their composition and the presence of minor elements. X-ray energy-dispersive spectrometry in the electron microscopes and mass spectrometry in the atom probe microscope showed that T1 ppts were enriched in zinc (Zn) and magnesium up to about 1.9 and 3.5 at.%, respectively. A concentration of 2.5 at.% Zn in the δ' ppts was also measured. Unlike Li and copper, Zn in the T1 ppts could not be detected using electron energy-loss spectroscopy in the transmission electron microscope because of its too low concentration and the small sizes of these ppts. Indeed, Monte Carlo simulations of EEL spectra for the Zn L2,3 edge showed that the signal-to-noise ratio was not high enough and that the detection limit was at least 2.5 at.%, depending on the probe current. Also, the simulation of X-ray spectra confirmed that the detection limit was exceeded for the Zn Kα X-ray line because the signal-to-noise ratio was high enough in that case, which is in agreement with our observations. © 2014 The Authors Journal of Microscopy © 2014 Royal Microscopical Society.

Coherent X-ray diffraction imaging of nanoengineered polymeric capsules

NASA Astrophysics Data System (ADS)

Erokhina, S.; Pastorino, L.; Di Lisa, D.; Kiiamov, A. G.; Faizullina, A. R.; Tayurskii, D. A.; Iannotta, S.; Erokhin, V.

2017-10-01

For the first time, nanoengineered polymeric capsules and their architecture have been studied with coherent X-ray diffraction imaging technique. The use of coherent X-ray diffraction imaging technique allowed us to analyze the samples immersed in a liquid. We report about the significant difference between polymeric capsule architectures under dry and liquid conditions.

Thermoelectric properties and thermal stability of Bi-doped PbTe single crystal

NASA Astrophysics Data System (ADS)

Chen, Zhong; Li, Decong; Deng, Shuping; Tang, Yu; Sun, Luqi; Liu, Wenting; Shen, Lanxian; Yang, Peizhi; Deng, Shukang

2018-06-01

In this study, n-type Bi-doped single-crystal PbTe thermoelectric materials were prepared by melting and slow cooling method according to the stoichiometric ratio of Pb:Bi:Te = 1-x:x:1 (x = 0, 0.1, 0.15, 0.2, 0.25). The X-ray diffraction patterns of Pb1-xBixTe samples show that all main diffraction peaks are well matched with the PbTe matrix, which has a face-centered cubic structure with the space group Fm 3 bar m . Electron probe microanalysis reveals that Pb content decreases gradually, and Te content remains invariant basically with the increase of Bi content, indicating that Bi atoms are more likely to replace Pb atoms. Thermal analysis shows that the prepared samples possess relatively high thermal stability. Simultaneously, transmission electron microscopy and selected area electron diffraction pattern indicate that the prepared samples have typical single-crystal structures with good mechanical properties. Moreover, the electrical conductivity of the prepared samples improved significantly compared with that of the pure sample, and the maximum ZT value of 0.84 was obtained at 600 K by the sample with x = 0.2.

Simultaneous neutron and x-ray imaging of inertial confinement fusion experiments along a single line of sight at Omega.

PubMed

Danly, C R; Day, T H; Fittinghoff, D N; Herrmann, H; Izumi, N; Kim, Y H; Martinez, J I; Merrill, F E; Schmidt, D W; Simpson, R A; Volegov, P L; Wilde, C H

2015-04-01

Neutron and x-ray imaging provide critical information about the geometry and hydrodynamics of inertial confinement fusion implosions. However, existing diagnostics at Omega and the National Ignition Facility (NIF) cannot produce images in both neutrons and x-rays along the same line of sight. This leads to difficulty comparing these images, which capture different parts of the plasma geometry, for the asymmetric implosions seen in present experiments. Further, even when opposing port neutron and x-ray images are available, they use different detectors and cannot provide positive information about the relative positions of the neutron and x-ray sources. A technique has been demonstrated on implosions at Omega that can capture x-ray images along the same line of sight as the neutron images. The technique is described, and data from a set of experiments are presented, along with a discussion of techniques for coregistration of the various images. It is concluded that the technique is viable and could provide valuable information if implemented on NIF in the near future.

Simultaneous neutron and x-ray imaging of inertial confinement fusion experiments along a single line of sight at Omega

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

Danly, C. R.; Day, T. H.; Fittinghoff, D. N.

Neutron and x-ray imaging provide critical information about the geometry and hydrodynamics of inertial confinement fusion implosions. However, existing diagnostics at Omega and the National Ignition Facility (NIF) cannot produce images in both neutrons and x-rays along the same line of sight. This leads to difficulty comparing these images, which capture different parts of the plasma geometry, for the asymmetric implosions seen in present experiments. Further, even when opposing port neutron and x-ray images are available, they use different detectors and cannot provide positive information about the relative positions of the neutron and x-ray sources. A technique has been demonstratedmore » on implosions at Omega that can capture x-ray images along the same line of sight as the neutron images. Thus, the technique is described, and data from a set of experiments are presented, along with a discussion of techniques for coregistration of the various images. It is concluded that the technique is viable and could provide valuable information if implemented on NIF in the near future.« less

Simultaneous neutron and x-ray imaging of inertial confinement fusion experiments along a single line of sight at Omega

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

Danly, C. R.; Day, T. H.; Herrmann, H.

Neutron and x-ray imaging provide critical information about the geometry and hydrodynamics of inertial confinement fusion implosions. However, existing diagnostics at Omega and the National Ignition Facility (NIF) cannot produce images in both neutrons and x-rays along the same line of sight. This leads to difficulty comparing these images, which capture different parts of the plasma geometry, for the asymmetric implosions seen in present experiments. Further, even when opposing port neutron and x-ray images are available, they use different detectors and cannot provide positive information about the relative positions of the neutron and x-ray sources. A technique has been demonstratedmore » on implosions at Omega that can capture x-ray images along the same line of sight as the neutron images. The technique is described, and data from a set of experiments are presented, along with a discussion of techniques for coregistration of the various images. It is concluded that the technique is viable and could provide valuable information if implemented on NIF in the near future.« less

Simultaneous neutron and x-ray imaging of inertial confinement fusion experiments along a single line of sight at Omega

DOE PAGES

Danly, C. R.; Day, T. H.; Fittinghoff, D. N.; ...

2015-04-16

Neutron and x-ray imaging provide critical information about the geometry and hydrodynamics of inertial confinement fusion implosions. However, existing diagnostics at Omega and the National Ignition Facility (NIF) cannot produce images in both neutrons and x-rays along the same line of sight. This leads to difficulty comparing these images, which capture different parts of the plasma geometry, for the asymmetric implosions seen in present experiments. Further, even when opposing port neutron and x-ray images are available, they use different detectors and cannot provide positive information about the relative positions of the neutron and x-ray sources. A technique has been demonstratedmore » on implosions at Omega that can capture x-ray images along the same line of sight as the neutron images. Thus, the technique is described, and data from a set of experiments are presented, along with a discussion of techniques for coregistration of the various images. It is concluded that the technique is viable and could provide valuable information if implemented on NIF in the near future.« less

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

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

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

2015-02-01

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

Physico-chemical analyses of Hispano-Moresque lustred ceramic: a precursor for Italian majolica?

NASA Astrophysics Data System (ADS)

Chabanne, D.; Bouquillon, A.; Aucouturier, M.; Dectot, X.; Padeletti, G.

2008-07-01

The paper presents a comprehensive physico-chemical investigation on a series of Hispano-Moresque objects produced in the eastern Spain workshops between the XIV and XVIII centuries and fragments from XII century, in order to compare them with the Italian Renaissance majolica production. The techniques used are mainly non-destructive (ion beam analyses and X-ray diffraction), sometimes complemented by SEM observation and microanalysis, and electrothermal atomic emission spectrometry. Such methods allow a full description of the terra cotta, of the glaze and of the different surface layers which constitute the lustre decoration indicating individual elemental composition and thickness of each layer containing or not metallic nanoparticles. Principal results show the following: i) a constant source of supply for the eastern Spain terra cotta; ii) a significant change in the composition of the Spanish glazes around the XVII century, with the disappearance of the opacifying tin oxide addition; iii) significant evolutions in the structure and composition of the lustre layers, in particular related to the presence or not of a metal-free surface glaze film and its thickness; iv) interesting analogies and differences with the Italian majolica; v) confirmation of the change in the quality of blue pigment during XVI century, already evidenced by the authors in previous publications. A discussion about the transmission of the lustre technique between eastern Spain and Italy at the Renaissance period is proposed.

Microanalysis study on ancient Wiangkalong Pottery

NASA Astrophysics Data System (ADS)

Won-in, K.; Tancharakorn, S.; Dararutana, P.

2017-09-01

Wiangkalong is one of major ceramic production cities in northern of Thailand, once colonized by the ancient Lanna Kingdom (1290 A.D.). Ancient Wiangkalong potteries were produced with shapes and designs as similar as those of the Chinese Yuan and Ming Dynasties. Due to the complex nature of materials and objects, extremely sensitive, spatially resolved, multi-elemental and versatile analytical instruments using non-destructive and non-sampling methods to analyze theirs composition are need. In this work, micro-beam X-ray fluorescence spectroscopy based on synchrotron radiation was firstly used to characterize the elemental composition of the ancient Wiangkalong pottery. The results showed the variations in elemental composition of the body matrix, the glaze and the underglaze painting, such as K, Ca, Ti, V, Cr, Mn and Fe.

An evaluation of smear layer with various desensitizing agents after tooth preparation.

PubMed

Zaimoglu, A; Aydin, A K

1992-09-01

According to hydrodynamics, any agent blocking the dentinal tubules reduces the flow of fluids and diminishes hypersensitivity. The properties of the desensitizing agents that sponsor tubular occlusion and the barrier efficiency resulting from the interaction of the smear layer with test materials were examined with the scanning electron microscope and energy-dispersive x-ray microanalysis. Selected dentinal desensitizing was accomplished with burnishing procedures, cavity varnish, calcium hydroxide, and topical fluoride. Subjective evaluations were also recorded clinically after tooth preparation. This investigation indicated that the smear layer did not protect against zinc phosphate cement, and that cavity varnish prevented the formation of the smear plugs. The smear layer and plugs were basically composed of calcium and phosphorus, the major ingredients of dentin.

3rd International Conference on X-ray Technique

NASA Astrophysics Data System (ADS)

Potrakhov, N. N.; Gryaznov, A. Yu; Lisenkov, A. A.; Kostrin, D. K.

2017-02-01

In this preface a brief history, modern aspects and future tendencies in development of the X-ray technique as seen from the 3rd International Conference on X-ray Technique that was held on 24-25 November 2016 in Saint Petersburg, Russia are described On 24-25 November 2016 in Saint Petersburg on the basis of Saint Petersburg State Electrotechnical University “LETI” n. a. V. I. Ulyanov (Lenin) was held the 3rd International Conference on X-ray Technique. The tradition to hold a similar conference in our country was laid in Soviet times. The last of them, the All-Union Conference on the Prospects of X-ray Tubes and Equipment was organized and held more than a quarter century ago - on 21-23 November 1999, at the initiative and under the leadership of the chief engineer of the Leningrad association of electronic industry “Svetlana” Borovsky Alexander Ivanovich and the chief of special design bureau of X-ray devices of “Svetlana” Shchukin Gennady Anatolievich. The most active part in the organization and work of the conference played members of the department of X-ray and electron beam instruments of Leningrad Electrotechnical Institute “LETI” (the former name of Saint Petersburg State Electrotechnical University “LETI”), represented by head of the department professor Ivanov Stanislav Alekseevich.

Grazing Incidence Wavefront Sensing and Verification of X-Ray Optics Performance

NASA Technical Reports Server (NTRS)

Saha, Timo T.; Rohrbach, Scott; Zhang, William W.

2011-01-01

Evaluation of interferometrically measured mirror metrology data and characterization of a telescope wavefront can be powerful tools in understanding of image characteristics of an x-ray optical system. In the development of soft x-ray telescope for the International X-Ray Observatory (IXO), we have developed new approaches to support the telescope development process. Interferometrically measuring the optical components over all relevant spatial frequencies can be used to evaluate and predict the performance of an x-ray telescope. Typically, the mirrors are measured using a mount that minimizes the mount and gravity induced errors. In the assembly and mounting process the shape of the mirror segments can dramatically change. We have developed wavefront sensing techniques suitable for the x-ray optical components to aid us in the characterization and evaluation of these changes. Hartmann sensing of a telescope and its components is a simple method that can be used to evaluate low order mirror surface errors and alignment errors. Phase retrieval techniques can also be used to assess and estimate the low order axial errors of the primary and secondary mirror segments. In this paper we describe the mathematical foundation of our Hartmann and phase retrieval sensing techniques. We show how these techniques can be used in the evaluation and performance prediction process of x-ray telescopes.

MMX-I: data-processing software for multimodal X-ray imaging and tomography.

PubMed

Bergamaschi, Antoine; Medjoubi, Kadda; Messaoudi, Cédric; Marco, Sergio; Somogyi, Andrea

2016-05-01

A new multi-platform freeware has been developed for the processing and reconstruction of scanning multi-technique X-ray imaging and tomography datasets. The software platform aims to treat different scanning imaging techniques: X-ray fluorescence, phase, absorption and dark field and any of their combinations, thus providing an easy-to-use data processing tool for the X-ray imaging user community. A dedicated data input stream copes with the input and management of large datasets (several hundred GB) collected during a typical multi-technique fast scan at the Nanoscopium beamline and even on a standard PC. To the authors' knowledge, this is the first software tool that aims at treating all of the modalities of scanning multi-technique imaging and tomography experiments.

Depth resolved compositional analysis of aluminium oxide thin film using non-destructive soft x-ray reflectivity technique

NASA Astrophysics Data System (ADS)

Sinha, Mangalika; Modi, Mohammed H.

2017-10-01

In-depth compositional analysis of 240 Å thick aluminium oxide thin film has been carried out using soft x-ray reflectivity (SXR) and x-ray photoelectron spectroscopy technique (XPS). The compositional details of the film is estimated by modelling the optical index profile obtained from the SXR measurements over 60-200 Å wavelength region. The SXR measurements are carried out at Indus-1 reflectivity beamline. The method suggests that the principal film region is comprised of Al2O3 and AlOx (x = 1.6) phases whereas the interface region comprised of SiO2 and AlOx (x = 1.6) mixture. The soft x-ray reflectivity technique combined with XPS measurements explains the compositional details of principal layer. Since the interface region cannot be analyzed with the XPS technique in a non-destructive manner in such a case the SXR technique is a powerful tool for nondestructive compositional analysis of interface region.

Ultrastructure of selected struvite-containing urinary calculi from cats.

PubMed

Neumann, R D; Ruby, A L; Ling, G V; Schiffman, P S; Johnson, D L

1996-01-01

To elucidate the ultrastructural details of struvite-containing urinary calculi from cats. Specimens studied were inclusive of the range of textures visible during preliminary analysis by use of a stereoscopic dissecting microscope. Textural types, which were used to infer crystal growth conditions, were differentiated with regard to crystal habit, crystal size, growth orientation, and primary porosity. Thirty specimens were selected from a collection of approximately 1,600 feline urinary calculi: 20 of these were composed entirely of struvite, and 10 consisted of struvite and calcium phosphate (apatite). Qualitative and quantitative analyses of specimens included use of plain and polarized light microscopy, x-ray diffractometry, scanning electron microscopy with backscattered electron imagery, x-ray fluorescence scans, and electron probe microanalysis. Four textural types were recognized among struvite calculi, whereas 2 textural types of struvite-apatite calculi were described. The presence of minute, well interconnected primary pores in struvite-containing urinary calculi from cats is an important feature, which may promote possible interaction of calculi with changes in urine composition. Primary porosity, which can facilitate interaction between the calculus and changing urine composition, may explain the efficacy of dietary or medicinal manipulations to promote the dissolution of struvite-containing uroliths from this species.

Lichens as environmental risk detectors

NASA Astrophysics Data System (ADS)

Caridi, F.; D'Agostino, M.; Messina, M.; Marcianò, G.; Grioli, L.; Belvedere, A.; Marguccio, S.; Belmusto, G.

2017-04-01

Several studies carried out after the Chernobyl nuclear accident in 1986 showed that lichens are suitable biomonitors of the fall-out, given their long life expectancy. 137Cs activity concentrations were measured through HPGe gamma spectrometry in different epiphytic lichens ( Usnea SPP, Platismatia glauca, Pseudevernia furfuracea, Ramalina SPP), collected from three sampling sites in the Calabria region, south of Italy. Data on variations in the contents of airborne particulates heavy metals, As, Be, Cd, Cu, Hg, Pb and Zn, measured in the thalli of the investigated lichens through inductively coupled plasma mass spectrometry (ICP-MS), were reported in accordance with a lichen thalli naturalness/alteration scale. Energy-dispersive X-ray microanalysis in a scanning electron microscope (SEM-EDX), with an electron beam of 20keV, that interacts with the sample leading to the emission of characteristic X-rays as secondary radiation, was also employed to investigate about the chemistry of the adherent particles to the surface of investigated lichens and about the possible interaction between them and the surrounding environment. Data obtained in this article provide useful information on the environmental risk of the studied area and can be further used for a radiological and chemical mapping.

Foliar manganese accumulation by Maytenus founieri (Celastraceae) in its native New Caledonian habitats: populational variation and localization by X-ray microanalysis.

PubMed

Fernando, D R; Woodrow, I E; Jaffré, T; Dumontet, V; Marshall, A T; Baker, A J M

2008-01-01

Hyperaccumulation by plants is a rare phenomenon that has potential practical benefits. The majority of manganese (Mn) hyperaccumulators discovered to date occur in New Caledonia, and little is known about their ecophysiology. This study reports on natural populations of one such species, the endemic shrub Maytenus founieri. Mean foliar Mn concentrations of two populations growing on ultramafic substrates with varying soil pHs were obtained. Leaf anatomies were examined by light microscopy, while the spatial distributions of foliar Mn in both populations were examined by qualitative scanning electron microscopy/energy dispersive spectroscopy (SEM/EDS). Plants growing on two different substrates were found to have very different mean dry weight (DW) foliar Mn concentrations. Light microscopy showed that the leaves had very distinct thick dermal structures, consisting of multiple layers of large cells in the hypodermis. In vivo X-ray microprobe analyses revealed that, in both populations, Mn sequestration occurred primarily in these dermal tissues. The finding here that foliar Mn is most highly localized in the nonphotosynthetic tissues of M. founieri contrasts with results from similar studies on other woody species that accumulate high Mn concentrations in their shoots.

Morphological changes of olivine grains reacted with amino acid solutions by impact process

NASA Astrophysics Data System (ADS)

Umeda, Yuhei; Takase, Atsushi; Fukunaga, Nao; Sekine, Toshimori; Kobayashi, Takamichi; Furukawa, Yoshihiro; Kakegawa, Takeshi

2017-03-01

Early oceans on Earth might have contained certain amounts of biomolecules such as amino acids, and they were subjected to meteorite impacts, especially during the late heavy bombardment. We performed shock recovery experiments by using a propellant gun in order to simulate shock reactions among olivine as a representative meteorite component, water and biomolecules in oceans in the process of marine meteorite impacts. In the present study, recovered solid samples were analyzed by using X-ray powder diffraction method, scanning electron microscopy, electron probe microanalysis, and transmission electron microscopy with energy-dispersive X-ray spectrometry. The analytical results on shocked products in the recovered sample showed (1) morphological changes of olivine to fiber- and bamboo shoot-like crystals, and to pulverized grains; and features of lumpy surfaces affected by hot water, (2) the formation of carbon-rich substances derived from amino acids, and (3) the incorporation of metals from container into samples. According to the present results, fine-grained olivine in meteorites might have morphologically changed and shock-induced chemical reactions might have been enhanced so that amino acids related to the origin of life may have transformed to carbon-rich substances by impacts.

Development and characterization of laser surface cladding (Ti,W)C reinforced Ni-30Cu alloy composite coating on copper

NASA Astrophysics Data System (ADS)

Yan, Hua; Zhang, Peilei; Yu, Zhishui; Li, Chonggui; Li, Ruidi

2012-07-01

To improve the wear resistance of copper components, laser surface cladding (LSC) was applied to deposit (Ti,W)C reinforced Ni-30Cu alloy composite coating on copper using a cladding interlayer of Ni-30Cu alloy by Nd:YAG laser. The microstructure and phases of the composite coating were investigated by scanning electron microscopy (SEM), X-ray diffraction (XRD) and X-ray energy dispersive microanalysis (EDX). Microhardness tester and pin-on-disc wear tester were employed to evaluate the hardness and dry-sliding wear resistance. The results show that crack-free composite coating with metallurgical bonding to the copper substrate is obtained. Phases identified in the (Ti,W)C-reinforced Ni-30Cu alloy composite layer are composed of TiWC2 reinforcements and (Ni,Cu) solid solution. TiWC2 reinforcements are distributed uniformly in the (Ni,Cu) solid solution matrix with dendritic morphology in the upper region and with particles in the mid-lower region. The microhardness and wear properties of the composite coating are improved significantly in comparison to the as-received copper substrate due to the addition of 50 wt% (Ti,W)C multicarbides.

Examination of Libby, Montana, Fill Material for Background Levels of Amphibole from the Rainy Creek Complex Using Scanning Electron Microscopy and X-Ray Microanalysis

USGS Publications Warehouse

Adams, David T.; Langer, William H.; Hoefen, Todd M.; Van Gosen, Bradley S.; Meeker, Gregory P.

2010-01-01

Natural background levels of Libby-type amphibole in the sediment of the Libby valley in Montana have not, up to this point, been determined. The purpose of this report is to provide the preliminary findings of a study designed by both the U.S. Geological Survey and the U.S. Environmental Protection Agency and performed by the U.S. Geological Survey. The study worked to constrain the natural background levels of fibrous amphiboles potentially derived from the nearby Rainy Creek Complex. The material selected for this study was sampled from three localities, two of which are active open-pit sand and gravel mines. Seventy samples were collected in total and examined using a scanning electron microscope equipped with an energy dispersive x-ray spectrometer. All samples contained varying amounts of feldspars, ilmenite, magnetite, quartz, clay minerals, pyroxene minerals, and non-fibrous amphiboles such as tremolite, actinolite, and magnesiohornblende. Of the 70 samples collected, only three had detectable levels of fibrous amphiboles compatible with those found in the rainy creek complex. The maximum concentration, identified here, of the amphiboles potentially from the Rainy Creek Complex is 0.083 percent by weight.

Characterization of leaf-level particulate matter for an industrial city using electron microscopy and X-ray microanalysis.

PubMed

Sgrigna, G; Baldacchini, C; Esposito, R; Calandrelli, R; Tiwary, A; Calfapietra, C

2016-04-01

This study reports application of monitoring and characterization protocol for particulate matter (PM) deposited on tree leaves, using Quercus ilex as a case study species. The study area is located in the industrial city of Terni in central Italy, with high PM concentrations. Four trees were selected as representative of distinct pollution environments based on their proximity to a steel factory and a street. Wash off from leaves onto cellulose filters were characterized using scanning electron microscopy and energy dispersive X-ray spectroscopy, inferring the associations between particle sizes, chemical composition, and sampling location. Modeling of particle size distributions showed a tri-modal fingerprint, with the three modes centered at 0.6 (factory related), 1.2 (urban background), and 2.6μm (traffic related). Chemical detection identified 23 elements abundant in the PM samples. Principal component analysis recognized iron and copper as source-specific PM markers, attributed mainly to industrial and heavy traffic pollution respectively. Upscaling these results on leaf area basis provided a useful indicator for strategic evaluation of harmful PM pollutants using tree leaves. Copyright © 2016. Published by Elsevier B.V.

Biosensor based on Prussian blue nanocubes/reduced graphene oxide nanocomposite for detection of organophosphorus pesticides

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

Zhang, Lin; Zhang, Aidong; Du, Dan

2012-07-13

We demonstrate a facile procedure to efficiently prepare Prussian blue nanocubes/reduced graphene oxide (PBNCs/rGO) nanocomposite by directly mixing Fe3+ and [Fe(CN)6]3 in the presence of GO in polyethyleneimine aqueous solution, resulting in a novel acetylcholinesterase (AChE) biosensor for detection of organophosphorus pesticides (OPs). The obtained nanocomposite was characterized by X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM) and energy dispersive X-ray (EDX) microanalysis. It was clearly observed that the nanosheet has been decorated with cubic PB nanoparticles and nearly all the nanoparticles are distributed uniformly only on the surface of the reduced GO. No isolated PB nanoparticles were observed, indicatingmore » the strong interaction between PB nanocubes and the reduced GO and the formation of PBNCs/rGO nanocomposite. The obtained PBNCs/rGO based AChE biosensor make the peak potential shift negatively to 220 mV. The AChE biosensor shows rapid response and high sensitivity for detection of monocrotophos. These results suggest that the PBNCs/rGO hybrids nanocomposite exhibited high electrocatalytic activity towards the oxidation of thiocholine, which lead to the sensitive detection of OP pesticides.« less

Facilities and Techniques for X-Ray Diagnostic Calibration in the 100-eV to 100-keV Energy Range

NASA Astrophysics Data System (ADS)

Gaines, J. L.; Wittmayer, F. J.

1986-08-01

The Lawrence Livermore National Laboratory (LLNL) has been a pioneer in the field of x-ray diagnostic calibration for more than 20 years. We have built steady state x-ray sources capable of supplying fluorescent lines of high spectral purity in the 100-eV to 100-keV energy range, and these sources have been used in the calibration of x-ray detectors, mirrors, crystals, filters, and film. This paper discusses our calibration philosophy and techniques, and describes some of our x-ray sources. Examples of actual calibration data are presented as well.

Nanoscience

DTIC Science & Technology

2011-07-22

L., Upgrading of Existing X - Ray Photoelectron Spectrometer Capabilities for Development and Analysis of Novel Energetic NanoCluster materials (DURIP...References From the Technical Reports database Allara, David L., Pennsylvania State University, Upgrading of Existing X - Ray Photoelectron...Scanning probe  X - ray Of these techniques, the most popularly used is the scanning probe, also known as the Dip-Pen Nanolithography (DPN) technique

A deterministic model of electron transport for electron probe microanalysis

NASA Astrophysics Data System (ADS)

Bünger, J.; Richter, S.; Torrilhon, M.

2018-01-01

Within the last decades significant improvements in the spatial resolution of electron probe microanalysis (EPMA) were obtained by instrumental enhancements. In contrast, the quantification procedures essentially remained unchanged. As the classical procedures assume either homogeneity or a multi-layered structure of the material, they limit the spatial resolution of EPMA. The possibilities of improving the spatial resolution through more sophisticated quantification procedures are therefore almost untouched. We investigate a new analytical model (M 1-model) for the quantification procedure based on fast and accurate modelling of electron-X-ray-matter interactions in complex materials using a deterministic approach to solve the electron transport equations. We outline the derivation of the model from the Boltzmann equation for electron transport using the method of moments with a minimum entropy closure and present first numerical results for three different test cases (homogeneous, thin film and interface). Taking Monte Carlo as a reference, the results for the three test cases show that the M 1-model is able to reproduce the electron dynamics in EPMA applications very well. Compared to classical analytical models like XPP and PAP, the M 1-model is more accurate and far more flexible, which indicates the potential of deterministic models of electron transport to further increase the spatial resolution of EPMA.

Improved electron probe microanalysis of trace elements in quartz

USGS Publications Warehouse

Donovan, John J.; Lowers, Heather; Rusk, Brian G.

2011-01-01

Quartz occurs in a wide range of geologic environments throughout the Earth's crust. The concentration and distribution of trace elements in quartz provide information such as temperature and other physical conditions of formation. Trace element analyses with modern electron-probe microanalysis (EPMA) instruments can achieve 99% confidence detection of ~100 ppm with fairly minimal effort for many elements in samples of low to moderate average atomic number such as many common oxides and silicates. However, trace element measurements below 100 ppm in many materials are limited, not only by the precision of the background measurement, but also by the accuracy with which background levels are determined. A new "blank" correction algorithm has been developed and tested on both Cameca and JEOL instruments, which applies a quantitative correction to the emitted X-ray intensities during the iteration of the sample matrix correction based on a zero level (or known trace) abundance calibration standard. This iterated blank correction, when combined with improved background fit models, and an "aggregate" intensity calculation utilizing multiple spectrometer intensities in software for greater geometric efficiency, yields a detection limit of 2 to 3 ppm for Ti and 6 to 7 ppm for Al in quartz at 99% t-test confidence with similar levels for absolute accuracy.

Large area soft x-ray collimator to facilitate x-ray optics testing

NASA Technical Reports Server (NTRS)

Espy, Samuel L.

1994-01-01

The first objective of this program is to design a nested conical foil x-ray optic which will collimate x-rays diverging from a point source. The collimator could then be employed in a small, inexpensive x-ray test stand which would be used to test various x-ray optics and detector systems. The second objective is to demonstrate the fabrication of the x-ray reflectors for this optic using lacquer-smoothing and zero-stress electroforming techniques.

Infrastructure development for radioactive materials at the NSLS-II

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

Sprouster, D. J.; Weidner, R.; Ghose, S. K.

2018-02-01

The X-ray Powder Diffraction (XPD) Beamline at the National Synchrotron Light Source-II is a multipurpose instrument designed for high-resolution, high-energy X-ray scattering techniques. In this article, the capabilities, opportunities and recent developments in the characterization of radioactive materials at XPD are described. The overarching goal of this work is to provide researchers access to advanced synchrotron techniques suited to the structural characterization of materials for advanced nuclear energy systems. XPD is a new beamline providing high photon flux for X-ray Diffraction, Pair Distribution Function analysis and Small Angle X-ray Scattering. The infrastructure and software described here extend the existing capabilitiesmore » at XPD to accommodate radioactive materials. Such techniques will contribute crucial information to the characterization and quantification of advanced materials for nuclear energy applications. We describe the automated radioactive sample collection capabilities and recent X-ray Diffraction and Small Angle X-ray Scattering results from neutron irradiated reactor pressure vessel steels and oxide dispersion strengthened steels.« less

Infrastructure development for radioactive materials at the NSLS-II

DOE PAGES

Sprouster, David J.; Weidner, R.; Ghose, S. K.; ...

2017-11-04

The X-ray Powder Diffraction (XPD) Beamline at the National Synchrotron Light Source-II is a multipurpose instrument designed for high-resolution, high-energy X-ray scattering techniques. In this paper, the capabilities, opportunities and recent developments in the characterization of radioactive materials at XPD are described. The overarching goal of this work is to provide researchers access to advanced synchrotron techniques suited to the structural characterization of materials for advanced nuclear energy systems. XPD is a new beamline providing high photon flux for X-ray Diffraction, Pair Distribution Function analysis and Small Angle X-ray Scattering. The infrastructure and software described here extend the existing capabilitiesmore » at XPD to accommodate radioactive materials. Such techniques will contribute crucial information to the characterization and quantification of advanced materials for nuclear energy applications. Finally, we describe the automated radioactive sample collection capabilities and recent X-ray Diffraction and Small Angle X-ray Scattering results from neutron irradiated reactor pressure vessel steels and oxide dispersion strengthened steels.« less

Fabricating Blazed Diffraction Gratings by X-Ray Lithography

NASA Technical Reports Server (NTRS)

Mouroulis, Pantazis; Hartley, Frank; Wilson, Daniel

2004-01-01

Gray-scale x-ray lithography is undergoing development as a technique for fabricating blazed diffraction gratings. As such, gray-scale x-ray lithography now complements such other grating-fabrication techniques as mechanical ruling, holography, ion etching, laser ablation, laser writing, and electron-beam lithography. Each of these techniques offers advantages and disadvantages for implementing specific grating designs; no single one of these techniques can satisfy the design requirements for all applications. Gray-scale x-ray lithography is expected to be advantageous for making gratings on steeper substrates than those that can be made by electron-beam lithography. This technique is not limited to sawtooth groove profiles and flat substrates: various groove profiles can be generated on arbitrarily shaped (including highly curved) substrates with the same ease as sawtooth profiles can be generated on flat substrates. Moreover, the gratings fabricated by this technique can be made free of ghosts (spurious diffraction components attributable to small spurious periodicities in the locations of grooves). The first step in gray-scale x-ray lithography is to conformally coat a substrate with a suitable photoresist. An x-ray mask (see Figure 1) is generated, placed between the substrate and a source of collimated x-rays, and scanned over the substrate so as to create a spatial modulation in the exposure of the photoresist. Development of the exposed photoresist results in a surface corrugation that corresponds to the spatial modulation and that defines the grating surface. The grating pattern is generated by scanning an appropriately shaped x-ray area mask along the substrate. The mask example of Figure 1 would generate a blazed grating profile when scanned in the perpendicular direction at constant speed, assuming the photoresist responds linearly to incident radiation. If the resist response is nonlinear, then the mask shape can be modified to account for the nonlinearity and produce a desired groove profile. An example of grating grooves generated by this technique is shown in Figure 2. A maximum relative efficiency of 88 percent has been demonstrated.

Towards simultaneous measurements of electronic and structural properties in ultra-fast x-ray free electron laser absorption spectroscopy experiments

NASA Astrophysics Data System (ADS)

Gaudin, J.; Fourment, C.; Cho, B. I.; Engelhorn, K.; Galtier, E.; Harmand, M.; Leguay, P. M.; Lee, H. J.; Nagler, B.; Nakatsutsumi, M.; Ozkan, C.; Störmer, M.; Toleikis, S.; Tschentscher, Th; Heimann, P. A.; Dorchies, F.

2014-04-01

The rapidly growing ultrafast science with X-ray lasers unveils atomic scale processes with unprecedented time resolution bringing the so called ``molecular movie'' within reach. X-ray absorption spectroscopy is one of the most powerful x-ray techniques providing both local atomic order and electronic structure when coupled with ad-hoc theory. Collecting absorption spectra within few x-ray pulses is possible only in a dispersive setup. We demonstrate ultrafast time-resolved measurements of the LIII-edge x-ray absorption near-edge spectra of irreversibly laser excited Molybdenum using an average of only few x-ray pulses with a signal to noise ratio limited only by the saturation level of the detector. The simplicity of the experimental set-up makes this technique versatile and applicable for a wide range of pump-probe experiments, particularly in the case of non-reversible processes.

Towards simultaneous measurements of electronic and structural properties in ultra-fast x-ray free electron laser absorption spectroscopy experiments

PubMed Central

Gaudin, J.; Fourment, C.; Cho, B. I.; Engelhorn, K.; Galtier, E.; Harmand, M.; Leguay, P. M.; Lee, H. J.; Nagler, B.; Nakatsutsumi, M.; Ozkan, C.; Störmer, M.; Toleikis, S.; Tschentscher, Th; Heimann, P. A.; Dorchies, F.

2014-01-01

The rapidly growing ultrafast science with X-ray lasers unveils atomic scale processes with unprecedented time resolution bringing the so called “molecular movie” within reach. X-ray absorption spectroscopy is one of the most powerful x-ray techniques providing both local atomic order and electronic structure when coupled with ad-hoc theory. Collecting absorption spectra within few x-ray pulses is possible only in a dispersive setup. We demonstrate ultrafast time-resolved measurements of the LIII-edge x-ray absorption near-edge spectra of irreversibly laser excited Molybdenum using an average of only few x-ray pulses with a signal to noise ratio limited only by the saturation level of the detector. The simplicity of the experimental set-up makes this technique versatile and applicable for a wide range of pump-probe experiments, particularly in the case of non-reversible processes. PMID:24740172

Towards simultaneous measurements of electronic and structural properties in ultra-fast x-ray free electron laser absorption spectroscopy experiments

DOE PAGES

Gaudin, J.; Fourment, C.; Cho, B. I.; ...

2014-04-17

The rapidly growing ultrafast science with X-ray lasers unveils atomic scale processes with unprecedented time resolution bringing the so called “molecular movie” within reach. X-ray absorption spectroscopy is one of the most powerful x-ray techniques providing both local atomic order and electronic structure when coupled with ad-hoc theory. Collecting absorption spectra within few x-ray pulses is possible only in a dispersive setup. We demonstrate ultrafast time-resolved measurements of the LIII-edge x-ray absorption near-edge spectra of irreversibly laser excited Molybdenum using an average of only few x-ray pulses with a signal to noise ratio limited only by the saturation level ofmore » the detector. The simplicity of the experimental set-up makes this technique versatile and applicable for a wide range of pump-probe experiments, particularly in the case of non-reversible processes.« less

Phase-sensitive X-ray imager

DOEpatents

Baker, Kevin Louis

2013-01-08

X-ray phase sensitive wave-front sensor techniques are detailed that are capable of measuring the entire two-dimensional x-ray electric field, both the amplitude and phase, with a single measurement. These Hartmann sensing and 2-D Shear interferometry wave-front sensors do not require a temporally coherent source and are therefore compatible with x-ray tubes and also with laser-produced or x-pinch x-ray sources.

Applications of synchrotron-based spectroscopic techniques in studying nucleic acids and nucleic acid-functionalized nanomaterials

PubMed Central

Wu, Peiwen; Yu, Yang; McGhee, Claire E.; Tan, Li Huey

2014-01-01

In this review, we summarize recent progresses in the application of synchrotron-based spectroscopic techniques for nucleic acid research that takes advantage of high-flux and high-brilliance electromagnetic radiation from synchrotron sources. The first section of the review focuses on the characterization of the structure and folding processes of nucleic acids using different types of synchrotron-based spectroscopies, such as X-ray absorption spectroscopy, X-ray emission spectroscopy, X-ray photoelectron spectroscopy, synchrotron radiation circular dichroism, X-ray footprinting and small-angle X-ray scattering. In the second section, the characterization of nucleic acid-based nanostructures, nucleic acid-functionalized nanomaterials and nucleic acid-lipid interactions using these spectroscopic techniques is summarized. Insights gained from these studies are described and future directions of this field are also discussed. PMID:25205057

Applications of synchrotron-based spectroscopic techniques in studying nucleic acids and nucleic acid-functionalized nanomaterials

DOE PAGES

Wu, Peiwen; Yu, Yang; McGhee, Claire E.; ...

2014-09-10

In this paper, we summarize recent progress in the application of synchrotron-based spectroscopic techniques for nucleic acid research that takes advantage of high-flux and high-brilliance electromagnetic radiation from synchrotron sources. The first section of the review focuses on the characterization of the structure and folding processes of nucleic acids using different types of synchrotron-based spectroscopies, such as X-ray absorption spectroscopy, X-ray emission spectroscopy, X-ray photoelectron spectroscopy, synchrotron radiation circular dichroism, X-ray footprinting and small-angle X-ray scattering. In the second section, the characterization of nucleic acid-based nanostructures, nucleic acid-functionalized nanomaterials and nucleic acid-lipid interactions using these spectroscopic techniques is summarized. Insightsmore » gained from these studies are described and future directions of this field are also discussed.« less

X-ray astronomical spectroscopy

NASA Technical Reports Server (NTRS)

Holt, Stephen S.

1987-01-01

The contributions of the Goddard group to the history of X-ray astronomy are numerous and varied. One role that the group has continued to play involves the pursuit of techniques for the measurement and interpretation of the X-ray spectra of cosmic sources. The latest development is the selection of the X-ray microcalorimeter for the Advanced X-ray Astrophysics Facility (AXAF) study payload. This technology is likely to revolutionize the study of cosmic X-ray spectra.

Use of different spectroscopic techniques in the analysis of Roman age wall paintings.

PubMed

Agnoli, Francesca; Calliari, Irene; Mazzocchin, Gian-Antonio

2007-01-01

In this paper the analysis of samples of Roman age wall paintings coming from: Pordenone, Vicenza and Verona is carried out by using three different techniques: energy dispersive x-rays spectroscopy (EDS), x-rays fluorescence (XRF) and proton induced x-rays emission (PIXE). The features of the three spectroscopic techniques in the analysis of samples of archaeological interest are discussed. The studied pigments were: cinnabar, yellow ochre, green earth, Egyptian blue and carbon black.

The effects of pre-ionization using a shunt resistor on reproducibility of the x-ray emission in a dense plasma focus device

NASA Astrophysics Data System (ADS)

Piriaei, D.; Yousefi, H. R.; Mahabadi, T. D.; SalarElahi, A.; Ghoranneviss, M.

2017-08-01

In this research, the effects of pre-ionization using a shunt resistor on reproducibility of x-ray emission in a Mather type plasma focus device have been studied. This technique increased the intensities of the emitted x-rays from argon as the filling gas of the device and made the x-ray yields with similar intensities reproducible. A Mirnov coil was also used to record the variations of the plasma's magnetic field, and the wavelet spectrums of these recorded signals showed the reduced instabilities due to the application of the pre-ionization technique. Moreover, it was demonstrated that this technique was capable of reducing the number of initial runaway electrons that could increase the impurities and instabilities inside the plasma. In addition to the above-mentioned features, this technique could improve the uniform formation of the current sheath during the breakdown phase that might later lead to a high quality pinch and high intensity emitted x-rays.

Quantitative X-ray Differential Interference Contrast Microscopy

NASA Astrophysics Data System (ADS)

Nakamura, Takashi

Full-field soft x-ray microscopes are widely used in many fields of sciences. Advances in nanofabrication technology enabled short wavelength focusing elements with significantly improved spatial resolution. In the soft x-ray spectral region, samples as small as 12 nm can be resolved using micro zone-plates as the objective lens. In addition to conventional x-ray microscopy in which x-ray absorption difference provides the image contrast, phase contrast mechanisms such as differential phase contrast (DIC) and Zernike phase contrast have also been demonstrated These phase contrast imaging mechanisms are especially attractive at the x-ray wavelengths where phase contrast of most materials is typically 10 times stronger than the absorption contrast. With recent progresses in plasma-based x- ray sources and increasing accessibility to synchrotron user facilities, x-ray microscopes are quickly becoming standard measurement equipment in the laboratory. To further the usefulness of x-ray DIC microscopy this thesis explicitly addresses three known issues with this imaging modality by introducing new techniques and devices First, as opposed to its visible-light counterpart, no quantitative phase imaging technique exists for x-ray DIC microscopy. To address this issue, two nanoscale x-ray quantitative phase imaging techniques, using exclusive OR (XOR) patterns and zone-plate doublets, respectively, are proposed. Unlike existing x-ray quantitative phase imaging techniques such as Talbot interferometry and ptychography, no dedicated experimental setups or stringent illumination coherence are needed for quantitative phase retrieval. Second, to the best of our knowledge, no quantitative performance characterization of DIC microscopy exists to date. Therefore the imaging system's response to sample's spatial frequency is not known In order to gain in-depth understanding of this imaging modality, performance of x-ray DIC microscopy is quantified using modulation transfer function. A new illumination apparatus required for the transfer function analysis under partially coherent illumination is also proposed. Such a characterization is essential for a proper selection of DIC optics for various transparent samples under study. Finally, optical elements used for x-ray DIC microscopy are highly absorptive and high brilliance x-ray sources such as synchrotrons are generally needed for image contrast. To extend the use of x-ray DIC microscopy to a wider variety of applications, a high efficiency large numerical aperture optical element consisting of high reflective Bragg reflectors is proposed. Using Bragg reflectors, which have 70% ˜99% reflectivity at extreme ultraviolet and soft x-rays for all angles of glancing incidence, the first order focusing efficiency is expected to increase by ˜ 8 times compared to that of a typical Fresnel zone-plate. This thesis contributes to current nanoscale x-ray phase contrast imaging research and provides new insights for biological, material, and magnetic sciences

Quantitative X-ray dark-field and phase tomography using single directional speckle scanning technique

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

Wang, Hongchang, E-mail: hongchang.wang@diamond.ac.uk; Kashyap, Yogesh; Sawhney, Kawal

2016-03-21

X-ray dark-field contrast tomography can provide important supplementary information inside a sample to the conventional absorption tomography. Recently, the X-ray speckle based technique has been proposed to provide qualitative two-dimensional dark-field imaging with a simple experimental arrangement. In this letter, we deduce a relationship between the second moment of scattering angle distribution and cross-correlation degradation of speckle and establish a quantitative basis of X-ray dark-field tomography using single directional speckle scanning technique. In addition, the phase contrast images can be simultaneously retrieved permitting tomographic reconstruction, which yields enhanced contrast in weakly absorbing materials. Such complementary tomography technique can allow systematicmore » investigation of complex samples containing both soft and hard materials.« less

MMX-I: data-processing software for multimodal X-ray imaging and tomography

PubMed Central

Bergamaschi, Antoine; Medjoubi, Kadda; Messaoudi, Cédric; Marco, Sergio; Somogyi, Andrea

2016-01-01

A new multi-platform freeware has been developed for the processing and reconstruction of scanning multi-technique X-ray imaging and tomography datasets. The software platform aims to treat different scanning imaging techniques: X-ray fluorescence, phase, absorption and dark field and any of their combinations, thus providing an easy-to-use data processing tool for the X-ray imaging user community. A dedicated data input stream copes with the input and management of large datasets (several hundred GB) collected during a typical multi-technique fast scan at the Nanoscopium beamline and even on a standard PC. To the authors’ knowledge, this is the first software tool that aims at treating all of the modalities of scanning multi-technique imaging and tomography experiments. PMID:27140159

Mononuclear Sulfido-Tungsten(V) Complexes: Completing the Tp*MEXY (M = Mo, W; E = O, S) Series.

PubMed

Sproules, Stephen; Eagle, Aston A; George, Graham N; White, Jonathan M; Young, Charles G

2017-05-01

Orange Tp*WSCl 2 has been synthesized from the reactions of Tp*WOCl 2 with boron sulfide in refluxing toluene or Tp*WS 2 Cl with PPh 3 in dichloromethane at room temperature. Mononuclear sulfido-tungsten(V) complexes, Tp*WSXY {X = Y = Cl, OPh, SPh, SePh; X = Cl, Y = OPh; XY = toluene-3,4-dithiolate (tdt), quinoxaline-2,3-dithiolate (qdt); and Tp* = hydrotris(3,5-dimethylpyrazol-1-yl)borate} were prepared by metathesis of Tp*WSCl 2 with the respective alkali metal salt of X - /XY 2- , or [NHEt 3 ] 2 (qdt). The complexes were characterized by microanalysis, mass spectrometry, electrochemistry, and infrared (IR), electron paramagnetic resonance (EPR) and electronic absorption spectroscopies. The molecular structures of Tp*WS(OPh) 2 , Tp*WS(SePh) 2 , and Tp*WS(tdt) have been determined by X-ray crystallography. The six-coordinate, distorted-octahedral W centers are coordinated by terminal sulfido (W≡S = 2.128(2) - 2.161(1) Å), terdentate facial Tp*, and monodentate/bidentate O/S/Se-donor ligands. The sulfido-W(V) complexes are characterized by lower energy electronic transitions, smaller g iso , and larger A iso ( 183 W) values, and more positive reduction potentials compared with their oxo-W(V) counterparts. This series has been probed by sulfur K-edge X-ray absorption spectroscopy (XAS), the spectra being assigned by comparison to Tp*WOXY (X = Y = SPh; XY = tdt, qdt) and time-dependent density functional theoretical (TD-DFT) calculations. This study provides insight into the electronic nature and chemistry of the catalytically and biologically important sulfido-W unit.

X-Ray Backscatter Imaging for Aerospace Applications

NASA Astrophysics Data System (ADS)

Shedlock, Daniel; Edwards, Talion; Toh, Chin

2011-06-01

Scatter x-ray imaging (SXI) is a real time, digital, x-ray backscatter imaging technique that allows radiographs to be taken from one side of an object. This x-ray backscatter imaging technique offers many advantages over conventional transmission radiography that include single-sided access and extremely low radiation fields compared to conventional open source industrial radiography. Examples of some applications include the detection of corrosion, foreign object debris, water intrusion, cracking, impact damage and leak detection in a variety of material such as aluminum, composites, honeycomb structures, and titanium.

X-ray phase contrast tomography by tracking near field speckle

PubMed Central

Wang, Hongchang; Berujon, Sebastien; Herzen, Julia; Atwood, Robert; Laundy, David; Hipp, Alexander; Sawhney, Kawal

2015-01-01

X-ray imaging techniques that capture variations in the x-ray phase can yield higher contrast images with lower x-ray dose than is possible with conventional absorption radiography. However, the extraction of phase information is often more difficult than the extraction of absorption information and requires a more sophisticated experimental arrangement. We here report a method for three-dimensional (3D) X-ray phase contrast computed tomography (CT) which gives quantitative volumetric information on the real part of the refractive index. The method is based on the recently developed X-ray speckle tracking technique in which the displacement of near field speckle is tracked using a digital image correlation algorithm. In addition to differential phase contrast projection images, the method allows the dark-field images to be simultaneously extracted. After reconstruction, compared to conventional absorption CT images, the 3D phase CT images show greatly enhanced contrast. This new imaging method has advantages compared to other X-ray imaging methods in simplicity of experimental arrangement, speed of measurement and relative insensitivity to beam movements. These features make the technique an attractive candidate for material imaging such as in-vivo imaging of biological systems containing soft tissue. PMID:25735237

X-ray microscopy of live biological micro-organisms

NASA Astrophysics Data System (ADS)

Raja Al-Ani, Ma'an Nassar

Real-time, compact x-ray microscopy has the potential to benefit many scientific fields, including microbiology, pharmacology, organic chemistry, and physics. Single frame x-ray micro-radiography, produced by a compact, solid-state laser plasma source, allows scientists to use x-ray emission for elemental analysis, and to observe biological specimens in their natural state. In this study, x-ray images of mouse kidney tissue, live bacteria, Pseudomonas aeruginosa and Burkholderia cepacia, and the bacteria's interaction with the antibiotic gentamicin, are examined using x-ray microscopy. For the purposes of comparing between confocal microscopy and x-ray microscopy, we introduced to our work the technique of gold labeling. Indirect immunofluorescence staining and immuno-gold labeling were applied on human lymphocytes and human tumor cells. Differential interference contrast microscopy (DIC) showed the lymphocyte body and nucleus, as did x-ray microscopy. However, the high resolution of x-ray microscopy allows us to differentiate between the gold particles bound to the antibodies and the free gold. A compact, tabletop Nd: glass laser is used in this study to produce x-rays from an Yttrium target. An atomic force microscope is used to scan the x-ray images from the developed photo-resist. The use of compact, tabletop laser plasma sources, in conjunction with x-ray microscopy, is a new technique that has great potential as a flexible, user-friendly scientific research tool.

A study of the x-ray image quality improvement in the examination of the respiratory system based on the new image processing technique

NASA Astrophysics Data System (ADS)

Nagai, Yuichi; Kitagawa, Mayumi; Torii, Jun; Iwase, Takumi; Aso, Tomohiko; Ihara, Kanyu; Fujikawa, Mari; Takeuchi, Yumiko; Suzuki, Katsumi; Ishiguro, Takashi; Hara, Akio

2014-03-01

Recently, the double contrast technique in a gastrointestinal examination and the transbronchial lung biopsy in an examination for the respiratory system [1-3] have made a remarkable progress. Especially in the transbronchial lung biopsy, better quality of x-ray fluoroscopic images is requested because this examination is performed under a guidance of x-ray fluoroscopic images. On the other hand, various image processing methods [4] for x-ray fluoroscopic images have been developed as an x-ray system with a flat panel detector [5-7] is widely used. A recursive filtering is an effective method to reduce a random noise in x-ray fluoroscopic images. However it has a limitation for its effectiveness of a noise reduction in case of a moving object exists in x-ray fluoroscopic images because the recursive filtering is a noise reduction method by adding last few images. After recursive filtering a residual signal was produced if a moving object existed in x-ray images, and this residual signal disturbed a smooth procedure of the examinations. To improve this situation, new noise reduction method has been developed. The Adaptive Noise Reduction [ANR] is the brand-new noise reduction technique which can be reduced only a noise regardless of the moving object in x-ray fluoroscopic images. Therefore the ANR is a very suitable noise reduction method for the transbronchial lung biopsy under a guidance of x-ray fluoroscopic images because the residual signal caused of the moving object in x-ray fluoroscopic images is never produced after the ANR. In this paper, we will explain an advantage of the ANR by comparing of a performance between the ANR images and the conventional recursive filtering images.

Hard and soft X-ray microscopy and tomography in catalysis: bridging the different time and length scales.

PubMed

Grunwaldt, Jan-Dierk; Schroer, Christian G

2010-12-01

X-ray microscopic techniques are excellent and presently emerging techniques for chemical imaging of heterogeneous catalysts. Spatially resolved studies in heterogeneous catalysis require the understanding of both the macro and the microstructure, since both have decisive influence on the final performance of the industrially applied catalysts. A particularly important aspect is the study of the catalysts during their preparation, activation and under operating conditions, where X-rays have an inherent advantage due to their good penetration length especially in the hard X-ray regime. Whereas reaction cell design for hard X-rays is straightforward, recently smart in situ cells have also been reported for the soft X-ray regime. In the first part of the tutorial review, the constraints from a catalysis view are outlined, then the scanning and full-field X-ray microscopy as well as coherent X-ray diffraction imaging techniques are described together with the challenging design of suitable environmental cells. Selected examples demonstrate the application of X-ray microscopy and tomography to monitor structural gradients in catalytic reactors and catalyst preparation with micrometre resolution but also the possibility to follow structural changes in the sub-100 nm regime. Moreover, the potential of the new synchrotron radiation sources with higher brilliance, recent milestones in focusing of hard X-rays as well as spatiotemporal studies are highlighted. The tutorial review concludes with a view on future developments in the field of X-ray microscopy that will have strong impact on the understanding of catalysts in the future and should be combined with in situ electron microscopic studies on the nanoscale and other spectroscopic studies like microRaman, microIR and microUV-vis on the macroscale.

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

PubMed

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

2012-04-03

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

Advanced x-ray imaging spectrometer

NASA Technical Reports Server (NTRS)

Callas, John L. (Inventor); Soli, George A. (Inventor)

1998-01-01

An x-ray spectrometer that also provides images of an x-ray source. Coded aperture imaging techniques are used to provide high resolution images. Imaging position-sensitive x-ray sensors with good energy resolution are utilized to provide excellent spectroscopic performance. The system produces high resolution spectral images of the x-ray source which can be viewed in any one of a number of specific energy bands.

X-Ray Nanofocus CT: Visualising Of Internal 3D-Structures With Submicrometer Resolution

NASA Astrophysics Data System (ADS)

Weinekoetter, Christian

2008-09-01

High-resolution X-ray Computed Tomography (CT) allows the visualization and failure analysis of the internal micro structure of objects—even if they have complicated 3D-structures where 2D X-ray microscopy would give unclear information. During the past several years, computed tomography has progressed to higher resolution and quicker reconstruction of the 3D-volume. Most recently it even allows a three-dimensional look into the inside of materials with submicron resolution. With the use of nanofocus® tube technology, nanoCT®-systems are pushing forward into application fields that were exclusive to high cost and rare available synchrotron techniques. The study was performed with the new nanotom, a very compact laboratory system which allows the analysis of samples up to 120 mm in diameter and weighing up to 1 kg with exceptional voxel-resolution down to <500 nm (<0.5 microns). It is the first 180 kV nanofocus® computed tomography system in the world which is tailored specifically to the highest-resolution applications in the fields of material science, micro electronics, geology and biology. Therefore it is particularly suitable for nanoCT-examinations e.g. of synthetic materials, metals, ceramics, composite materials, mineral and organic samples. There are a few physical effects influencing the CT quality, such as beam-hardening within the sample or ring-artefacts, which can not be completely avoided. To optimize the quality of high resolution 3D volumes, the nanotom® includes a variety of effective software tools to reduce ring-artefacts and correct beam hardenings or drift effects which occurred during data acquisition. The resulting CT volume data set can be displayed in various ways, for example by virtual slicing and sectional views in any direction of the volume. By the fact that this requires only a mouse click, this technique will substitute destructive mechanical slicing and cutting in many applications. The initial CT results obtained with the nanotom® demonstrate that it is now possible to analyze the three-dimensional micro structure of materials and small objects with submicrometer resolution. Any internal difference in material, density or porosity within a sample can be visualized and data like distances can be measured. NanoCT® widely expands the spectrum of detectable micro-structures. The nanotom® opens a new dimension of 3D-microanalysis and will replace more destructive methods—saving costs and time per sample inspected.

X-ray near-field speckle: implementation and critical analysis

PubMed Central

Lu, Xinhui; Mochrie, S. G. J.; Narayanan, S.; Sandy, A. R.; Sprung, M.

2011-01-01

The newly introduced coherence-based technique of X-ray near-field speckle (XNFS) has been implemented at 8-ID-I at the Advanced Photon Source. In the near-field regime of high-brilliance synchrotron X-rays scattered from a sample of interest, it turns out that, when the scattered radiation and the main beam both impinge upon an X-ray area detector, the measured intensity shows low-contrast speckles, resulting from interference between the incident and scattered beams. A micrometer-resolution XNFS detector with a high numerical aperture microscope objective has been built and its capability for studying static structures and dynamics at longer length scales than traditional far-field X-ray scattering techniques is demonstrated. Specifically, the dynamics of dilute silica and polystyrene colloidal samples are characterized. This study reveals certain limitations of the XNFS technique, especially in the characterization of static structures, which is discussed. PMID:21997906

Correlation between protein sequence similarity and x-ray diffraction quality in the protein data bank.

PubMed

Lu, Hui-Meng; Yin, Da-Chuan; Ye, Ya-Jing; Luo, Hui-Min; Geng, Li-Qiang; Li, Hai-Sheng; Guo, Wei-Hong; Shang, Peng

2009-01-01

As the most widely utilized technique to determine the 3-dimensional structure of protein molecules, X-ray crystallography can provide structure of the highest resolution among the developed techniques. The resolution obtained via X-ray crystallography is known to be influenced by many factors, such as the crystal quality, diffraction techniques, and X-ray sources, etc. In this paper, the authors found that the protein sequence could also be one of the factors. We extracted information of the resolution and the sequence of proteins from the Protein Data Bank (PDB), classified the proteins into different clusters according to the sequence similarity, and statistically analyzed the relationship between the sequence similarity and the best resolution obtained. The results showed that there was a pronounced correlation between the sequence similarity and the obtained resolution. These results indicate that protein structure itself is one variable that may affect resolution when X-ray crystallography is used.

Nanosecond time resolved x-ray diagnostics of relativistic electron beam initiated events

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

Kuswa, Glenn W.; Chang, James

The dynamic behavior of a test sample during aid shortly after it has teen irradiated by an intense relativistic electron beam (REB) is of great interest to the study of team energy deposition. Since the sample densities are far beyond the cutoff in the optical region, flash x-radiography techniques have been developed to diagnose the evolution of the samples. The conventional approach of analyzing the dynamic behavior of solid densities utilizes one or more short x-ray bursts to record images on photographic emulsion. This technique is not useful in the presence of the intense x-rays from the REB interacting withmore » the sample. We report two techniques for isolating the film package from the REB x-ray pulse.« less

Motionless phase stepping in X-ray phase contrast imaging with a compact source

PubMed Central

Miao, Houxun; Chen, Lei; Bennett, Eric E.; Adamo, Nick M.; Gomella, Andrew A.; DeLuca, Alexa M.; Patel, Ajay; Morgan, Nicole Y.; Wen, Han

2013-01-01

X-ray phase contrast imaging offers a way to visualize the internal structures of an object without the need to deposit significant radiation, and thereby alleviate the main concern in X-ray diagnostic imaging procedures today. Grating-based differential phase contrast imaging techniques are compatible with compact X-ray sources, which is a key requirement for the majority of clinical X-ray modalities. However, these methods are substantially limited by the need for mechanical phase stepping. We describe an electromagnetic phase-stepping method that eliminates mechanical motion, thus removing the constraints in speed, accuracy, and flexibility. The method is broadly applicable to both projection and tomography imaging modes. The transition from mechanical to electromagnetic scanning should greatly facilitate the translation of X-ray phase contrast techniques into mainstream applications. PMID:24218599

Collection of wood quality data by X-ray densitometry: a case study with three southern pines

Treesearch

Thomas L. Eberhardt; Lisa J. Samuelson

2015-01-01

X-ray densitometry is a technique often used in tree growth and wood quality studies to incrementally measure density (specific gravity) along a radial strip of wood. Protocols for this technique vary between laboratories because of differences in species, equipment, tree age, and other factors. Here, the application of X-ray densitometry is discussed in terms of a...

X-ray imaging for studying behavior of liquids at high pressures and high temperatures using Paris-Edinburgh press.

PubMed

Kono, Yoshio; Kenney-Benson, Curtis; Shibazaki, Yuki; Park, Changyong; Wang, Yanbin; Shen, Guoyin

2015-07-01

Several X-ray techniques for studying structure, elastic properties, viscosity, and immiscibility of liquids at high pressures have been integrated using a Paris-Edinburgh press at the 16-BM-B beamline of the Advanced Photon Source. Here, we report the development of X-ray imaging techniques suitable for studying behavior of liquids at high pressures and high temperatures. White X-ray radiography allows for imaging phase separation and immiscibility of melts at high pressures, identified not only by density contrast but also by phase contrast imaging in particular for low density contrast liquids such as silicate and carbonate melts. In addition, ultrafast X-ray imaging, at frame rates up to ∼10(5) frames/second (fps) in air and up to ∼10(4) fps in Paris-Edinburgh press, enables us to investigate dynamics of liquids at high pressures. Very low viscosities of melts similar to that of water can be reliably measured. These high-pressure X-ray imaging techniques provide useful tools for understanding behavior of liquids or melts at high pressures and high temperatures.

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

NASA Astrophysics Data System (ADS)

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

2016-10-01

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

Development of XAFS Into a Structure Determination Technique

NASA Astrophysics Data System (ADS)

Stern, E. A.

After the detection of diffraction of x-rays by M. Laue in 1912, the technique was soon applied to structure determination by Bragg within a year. On the other hand, although the edge steps in X-Ray absorption were discovered even earlier by Barkla and both the near edge (XANES) and extended X-Ray fine structure (EXAFS) past the edge were detected by 1929, it still took over 40 years to realize the structure information contained in this X-Ray absorption fine structure (XAFS). To understand this delay a brief historical review of the development of the scientific ideas that transformed XAFS into the premiere technique for local structure determination is given. The development includes both advances in theoretical understanding and calculational capabilities, and in experimental facilities, especially synchrotron radiation sources. The present state of the XAFS technique and its capabilities are summarized.

Characterization of ion beam sputtered deposited W/Si multilayers by grazing incidence x-ray diffraction and x-ray reflectivity technique

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

Dhawan, Rajnish, E-mail: rajnish@rrcat.gov.in; Rai, Sanjay

2016-05-23

W/Si multilayers four samples have been deposited on silicon substrate using ion beam sputtering system. Thickness of tungsten (W) varies from around 10 Å to 40 Å while the silicon (Si) thickness remains constant at around 30 Å in multilayers [W-Si]{sub x4}. The samples have been characterized by grazing incidence X-ray diffraction (GIXRD) and X-ray reflectivity technique (XRR). GIXRD study shows the crystalline behaviour of W/Si multilayer by varying W thickness and it is found that above 20 Å the W film transform from amorphous to crystalline phase and X-ray reflectivity data shows that the roughnesses of W increases onmore » increasing the W thicknesses in W/Si multilayers.« less

Advances in functional X-ray imaging techniques and contrast agents

PubMed Central

Chen, Hongyu; Rogalski, Melissa M.

2012-01-01

X-rays have been used for non-invasive high-resolution imaging of thick biological specimens since their discovery in 1895. They are widely used for structural imaging of bone, metal implants, and cavities in soft tissue. Recently, a number of new contrast methodologies have emerged which are expanding X-ray’s biomedical applications to functional as well as structural imaging. These techniques are promising to dramatically improve our ability to study in situ biochemistry and disease pathology. In this review, we discuss how X-ray absorption, X-ray fluorescence, and X-ray excited optical luminescence can be used for physiological, elemental, and molecular imaging of vasculature, tumours, pharmaceutical distribution, and the surface of implants. Imaging of endogenous elements, exogenous labels, and analytes detected with optical indicators will be discussed. PMID:22962667

Synchrotron Radiation X-ray Diffraction Techniques Applied to Insect Flight Muscle.

PubMed

Iwamoto, Hiroyuki

2018-06-13

X-ray fiber diffraction is a powerful tool used for investigating the molecular structure of muscle and its dynamics during contraction. This technique has been successfully applied not only to skeletal and cardiac muscles of vertebrates but also to insect flight muscle. Generally, insect flight muscle has a highly ordered structure and is often capable of high-frequency oscillations. The X-ray diffraction studies on muscle have been accelerated by the advent of 3rd-generation synchrotron radiation facilities, which can generate brilliant and highly oriented X-ray beams. This review focuses on some of the novel experiments done on insect flight muscle by using synchrotron radiation X-rays. These include diffraction recordings from single myofibrils within a flight muscle fiber by using X-ray microbeams and high-speed diffraction recordings from the flight muscle during the wing-beat of live insects. These experiments have provided information about the molecular structure and dynamic function of flight muscle in unprecedented detail. Future directions of X-ray diffraction studies on muscle are also discussed.

Alignment and Integration Techniques for Mirror Segment Pairs on the Constellation X Telescope

NASA Technical Reports Server (NTRS)

Hadjimichael, Theo; Lehan, John; Olsen, Larry; Owens, Scott; Saha, Timo; Wallace, Tom; Zhang, Will

2007-01-01

We present the concepts behind current alignment and integration techniques for testing a Constellation-X primary-secondary mirror segment pair in an x-ray beam line test. We examine the effects of a passive mount on thin glass x-ray mirror segments, and the issues of mount shape and environment on alignment. We also investigate how bonding and transfer to a permanent housing affects the quality of the final image, comparing predicted results to a full x-ray test on a primary secondary pair.

Enhanced ionic conductivity in planar sodium-β"-alumina electrolyte for electrochemical energy storage applications.

PubMed

La Rosa, Daniela; Monforte, Giuseppe; D'Urso, Claudia; Baglio, Vincenzo; Antonucci, Vincenzo; Aricò, Antonino S

2010-12-17

Solid Na-β"-Al₂O₃ electrolyte is prepared by a simple chemical route involving a pseudo-boehmite precursor and thermal treatment. Boehmite powder is used for manufacturing the planar electrolyte with appropriate bulk density after firing at 1500 °C. The structure, morphology, and surface properties of precursor powders and sintered electrolytes are investigated by X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), and X-ray photoelectron spectroscopy (XPS). As shown by XRD and TEM analyses, nanometer-sized particles are obtained for the boehmite precursor and a pure crystallographic phase is achieved for the sintered electrolyte. SEM analysis of the cross-section indicates good sintering characteristics. XPS shows a higher Na/Al atomic ratio on the surface for the planar electrolyte compared to a commercial tubular electrolyte (0.57 vs. 0.46). Energy-dispersive X-ray microanalysis (EDX) shows an Na/Al ratio in the bulk of 0.16, similar in the two samples. The ionic conductivity of the planar electrolyte is larger than that measured on a commercial tube of sodium-β"-alumina in a wide temperature range. At 350 °C, conductivity values of 0.5 S cm⁻¹ and 0.26 S cm⁻¹ are obtained for the planar electrolyte and the commercial tube, respectively. AC-impedance spectra show smaller grain boundary effects in the planar electrolyte than in the tubular electrolyte. These favorable properties may increase the perspectives for applying planar Na-β"-Al₂O₃ electrolytes in high-temperature batteries.

Effects of rare earth doping on multi-core iron oxide nanoparticles properties

NASA Astrophysics Data System (ADS)

Petran, Anca; Radu, Teodora; Borodi, Gheorghe; Nan, Alexandrina; Suciu, Maria; Turcu, Rodica

2018-01-01

New multi-core iron oxide magnetic nanoparticles doped with rare earth metals (Gd, Eu) were obtained by a one step synthesis procedure using a solvothermal method for potential biomedical applications. The obtained clusters were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), energy-dispersive X-ray microanalysis (EDX), X-ray photoelectron spectroscopy (XPS) and magnetization measurements. They possess high colloidal stability, a saturation magnetization of up to 52 emu/g, and nearly spherical shape. The presence of rare earth ions in the obtained samples was confirmed by EDX and XPS. XRD analysis proved the homogeneous distribution of the trivalent rare earth ions in the inverse-spinel structure of magnetite and the increase of crystal strain upon doping the samples. XPS study reveals the valence state and the cation distribution on the octahedral and tetrahedral sites of the analysed samples. The observed shift of the XPS valence band spectra maximum in the direction of higher binding energies after rare earth doping, as well as theoretical valence band calculations prove the presence of Gd and Eu ions in octahedral sites. The blood protein adsorption ability of the obtained samples surface, the most important factor of the interaction between biomaterials and body fluids, was assessed by interaction with bovine serum albumin (BSA). The rare earth doped clusters surface show higher afinity for binding BSA. In vitro cytotoxicity test results for the studied samples showed no cytotoxicity in low and medium doses, establishing a potential perspective for rare earth doped MNC to facilitate multiple therapies in a single formulation for cancer theranostics.

Rise time measurement for ultrafast X-ray pulses

DOEpatents

Celliers, Peter M [Berkeley, CA; Weber, Franz A [Oakland, CA; Moon, Stephen J [Tracy, CA

2005-04-05

A pump-probe scheme measures the rise time of ultrafast x-ray pulses. Conventional high speed x-ray diagnostics (x-ray streak cameras, PIN diodes, diamond PCD devices) do not provide sufficient time resolution to resolve rise times of x-ray pulses on the order of 50 fs or less as they are being produced by modern fast x-ray sources. Here, we are describing a pump-probe technique that can be employed to measure events where detector resolution is insufficient to resolve the event. The scheme utilizes a diamond plate as an x-ray transducer and a p-polarized probe beam.

Rise Time Measurement for Ultrafast X-Ray Pulses

DOEpatents

Celliers, Peter M.; Weber, Franz A.; Moon, Stephen J.

2005-04-05

A pump-probe scheme measures the rise time of ultrafast x-ray pulses. Conventional high speed x-ray diagnostics (x-ray streak cameras, PIN diodes, diamond PCD devices) do not provide sufficient time resolution to resolve rise times of x-ray pulses on the order of 50 fs or less as they are being produced by modern fast x-ray sources. Here, we are describing a pump-probe technique that can be employed to measure events where detector resolution is insufficient to resolve the event. The scheme utilizes a diamond plate as an x-ray transducer and a p-polarized probe beam.

Nanoscale characterization of local structures and defects in photonic crystals using synchrotron-based transmission soft X-ray microscopy

PubMed Central

Nho, Hyun Woo; Kalegowda, Yogesh; Shin, Hyun-Joon; Yoon, Tae Hyun

2016-01-01

For the structural characterization of the polystyrene (PS)-based photonic crystals (PCs), fast and direct imaging capabilities of full field transmission X-ray microscopy (TXM) were demonstrated at soft X-ray energy. PS-based PCs were prepared on an O2-plasma treated Si3N4 window and their local structures and defects were investigated using this label-free TXM technique with an image acquisition speed of ~10 sec/frame and marginal radiation damage. Micro-domains of face-centered cubic (FCC (111)) and hexagonal close-packed (HCP (0001)) structures were dominantly found in PS-based PCs, while point and line defects, FCC (100), and 12-fold symmetry structures were also identified as minor components. Additionally, in situ observation capability for hydrated samples and 3D tomographic reconstruction of TXM images were also demonstrated. This soft X-ray full field TXM technique with faster image acquisition speed, in situ observation, and 3D tomography capability can be complementally used with the other X-ray microscopic techniques (i.e., scanning transmission X-ray microscopy, STXM) as well as conventional characterization methods (e.g., electron microscopic and optical/fluorescence microscopic techniques) for clearer structure identification of self-assembled PCs and better understanding of the relationship between their structures and resultant optical properties. PMID:27087141

Correlative analysis of hard and soft x ray observations of solar flares

NASA Technical Reports Server (NTRS)

Zarro, Dominic M.

1994-01-01

We have developed a promising new technique for jointly analyzing BATSE hard X-ray observations of solar flares with simultaneous soft X-ray observations. The technique is based upon a model in which electric currents and associated electric fields are responsible for the respective heating and particle acceleration that occur in solar flares. A useful by-product of this technique is the strength and evolution of the coronal electric field. The latter permits one to derive important flare parameters such as the current density, the number of current filaments composing the loop, and ultimately the hard X-ray spectrum produced by the runaway electrons. We are continuing to explore the technique by applying it to additional flares for which we have joint BATSE/Yohkoh observations. A central assumption of our analysis is the constant of proportionality alpha relating the hard X-ray flux above 50 keV and the rate of electron acceleration. For a thick-target model of hard X-ray production, it can be shown that cv is in fact related to the spectral index and low-energy cutoff of precipitating electrons. The next step in our analysis is to place observational constraints on the latter parameters using the joint BATSE/Yohkoh data.

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

Ovcharov, A. V.; Karateev, I. A.; Mikhutkin, A. A.

The surface microstructure of Ni–W alloy tapes, which are used as substrates to form films of high-temperature superconductors and photovoltaic devices, has been studied. Several samples of a Ni{sub 95}W{sub 5} tape (Evico) annealed under different conditions were analyzed using scanning electron microscopy, energy-dispersive X-ray microanalysis, electron diffraction, and electron energy-loss spectroscopy. NiWO{sub 4} precipitates are found on the surface of annealed samples. The growth of precipitates at a temperature of 950°C is accompanied by the formation of pores on the surface or under an oxide film. Depressions with a wedge-shaped profile are found at the grain boundaries. Annealing inmore » a reducing atmosphere using a specially prepared chamber allows one to form a surface free of nickel tungstate precipitates.« less

Ultrastructural effects on gill tissues induced in red tilapia Oreochromis sp. by a waterborne lead exposure.

PubMed

Aldoghachi, Mohammed A; Azirun, Mohd Sofian; Yusoff, Ismail; Ashraf, Muhammad Aqeel

2016-09-01

Experiments on hybrid red tilapia Oreochromis sp. were conducted to assess histopathological effects induced in gill tissues of 96 h exposure to waterborne lead (5.5 mg/L). These tissues were investigated by light and scanning electron microscopy. Results showed that structural design of gill tissues was noticeably disrupted. Major symptoms were changes of epithelial cells, fusion in adjacent secondary lamellae, hypertrophy and hyperplasia of chloride cells and coagulate necrosis in pavement cells with disappearance of its microridges. Electron microscopic X-ray microanalysis of fish gills exposed to sublethal lead revealed that lead accumulated on the surface of the gill lamella. This study confirmed that lead exposure incited a difference of histological impairment in fish, supporting environmental watch over aquatic systems when polluted by lead.

"Cold" synthesis of carbon from polyvinyl chloride with the use of an electron beam ejected into the atmosphere

NASA Astrophysics Data System (ADS)

Kryazhev, Yu. G.; Vorob'ev, M. S.; Koval', N. N.; Trenikhin, M. V.; Solodovnichenko, V. S.; Sulakshin, S. A.; Likholobov, V. A.

2016-10-01

This work shows the possibility in principle of forming hydrocarbon structures in polyvinyl chloride films free of admixtures and polyvinyl chloride films modified with 5-mass % ferrocene via a radiation chemical transformation in the atmosphere with the use of an electron accelerator with a plasma cathode operating in the pulsed-periodic mode maximal electron energy no higher than 160 keV, pulse length of 40 μs, and current density of 5 mA/cm2. According to the results of semiquantitative X-ray microanalysis, an irradiated polyvinyl chloride film free of admixtures contains 92 of carbon, 6 of oxygen, and 2 mass % of chlorine; the irradiated polyvinyl chloride is an amorphous carbon material. A possible mechanism of the phenomenon is discussed.

Speckle-based at-wavelength metrology of X-ray mirrors with super accuracy

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

Kashyap, Yogesh; Wang, Hongchang; Sawhney, Kawal, E-mail: kawal.sawhney@diamond.ac.uk

2016-05-15

X-ray active mirrors, such as bimorph and mechanically bendable mirrors, are increasingly being used on beamlines at modern synchrotron source facilities to generate either focused or “tophat” beams. As well as optical tests in the metrology lab, it is becoming increasingly important to optimise and characterise active optics under actual beamline operating conditions. Recently developed X-ray speckle-based at-wavelength metrology technique has shown great potential. The technique has been established and further developed at the Diamond Light Source and is increasingly being used to optimise active mirrors. Details of the X-ray speckle-based at-wavelength metrology technique and an example of its applicabilitymore » in characterising and optimising a micro-focusing bimorph X-ray mirror are presented. Importantly, an unprecedented angular sensitivity in the range of two nanoradians for measuring the slope error of an optical surface has been demonstrated. Such a super precision metrology technique will be beneficial to the manufacturers of polished mirrors and also in optimization of beam shaping during experiments.« less

Radiation exposure in X-ray-based imaging techniques used in osteoporosis

PubMed Central

Adams, Judith E.; Guglielmi, Giuseppe; Link, Thomas M.

2010-01-01

Recent advances in medical X-ray imaging have enabled the development of new techniques capable of assessing not only bone quantity but also structure. This article provides (a) a brief review of the current X-ray methods used for quantitative assessment of the skeleton, (b) data on the levels of radiation exposure associated with these methods and (c) information about radiation safety issues. Radiation doses associated with dual-energy X-ray absorptiometry are very low. However, as with any X-ray imaging technique, each particular examination must always be clinically justified. When an examination is justified, the emphasis must be on dose optimisation of imaging protocols. Dose optimisation is more important for paediatric examinations because children are more vulnerable to radiation than adults. Methods based on multi-detector CT (MDCT) are associated with higher radiation doses. New 3D volumetric hip and spine quantitative computed tomography (QCT) techniques and high-resolution MDCT for evaluation of bone structure deliver doses to patients from 1 to 3 mSv. Low-dose protocols are needed to reduce radiation exposure from these methods and minimise associated health risks. PMID:20559834

A detailed study of gold-nanoparticle loaded cells using X-ray based techniques for cell-tracking applications with single-cell sensitivity

NASA Astrophysics Data System (ADS)

Astolfo, Alberto; Arfelli, Fulvia; Schültke, Elisabeth; James, Simon; Mancini, Lucia; Menk, Ralf-Hendrik

2013-03-01

In the present study complementary high-resolution imaging techniques on different length scales are applied to elucidate a cellular loading protocol of gold nanoparticles and subsequently its impact on long term and high-resolution cell-tracking utilizing X-ray technology. Although demonstrated for malignant cell lines the results can be applied to non-malignant cell lines as well. In particular the accumulation of the gold marker per cell has been assessed quantitatively by virtue of electron microscopy, two-dimensional X-ray fluorescence imaging techniques and X-ray CT with micrometric and sub-micrometric resolution. Moreover, utilizing these techniques the three dimensional distribution of the incorporated nanoparticles, which are sequestered in lysosomes as a permanent marker, could be determined. The latter allowed elucidation of the gold partition during mitosis and the cell size, which subsequently enabled us to define the optimal instrument settings of a compact microCT system to visualize gold loaded cells. The results obtained demonstrate the feasibility of cell-tracking using X-ray CT with compact sources.

3D X-ray ultra-microscopy of bone tissue.

PubMed

Langer, M; Peyrin, F

2016-02-01

We review the current X-ray techniques with 3D imaging capability at the nano-scale: transmission X-ray microscopy, ptychography and in-line phase nano-tomography. We further review the different ultra-structural features that have so far been resolved: the lacuno-canalicular network, collagen orientation, nano-scale mineralization and their use as basis for mechanical simulations. X-ray computed tomography at the micro-metric scale is increasingly considered as the reference technique in imaging of bone micro-structure. The trend has been to push towards increasingly higher resolution. Due to the difficulty of realizing optics in the hard X-ray regime, the magnification has mainly been due to the use of visible light optics and indirect detection of the X-rays, which limits the attainable resolution with respect to the wavelength of the visible light used in detection. Recent developments in X-ray optics and instrumentation have allowed to implement several types of methods that achieve imaging that is limited in resolution by the X-ray wavelength, thus enabling computed tomography at the nano-scale. We review here the X-ray techniques with 3D imaging capability at the nano-scale: transmission X-ray microscopy, ptychography and in-line phase nano-tomography. Further, we review the different ultra-structural features that have so far been resolved and the applications that have been reported: imaging of the lacuno-canalicular network, direct analysis of collagen orientation, analysis of mineralization on the nano-scale and use of 3D images at the nano-scale to drive mechanical simulations. Finally, we discuss the issue of going beyond qualitative description to quantification of ultra-structural features.

Combining X-ray and neutron crystallography with spectroscopy.

PubMed

Kwon, Hanna; Smith, Oliver; Raven, Emma Lloyd; Moody, Peter C E

2017-02-01

X-ray protein crystallography has, through the determination of the three-dimensional structures of enzymes and their complexes, been essential to the understanding of biological chemistry. However, as X-rays are scattered by electrons, the technique has difficulty locating the presence and position of H atoms (and cannot locate H + ions), knowledge of which is often crucially important for the understanding of enzyme mechanism. Furthermore, X-ray irradiation, through photoelectronic effects, will perturb the redox state in the crystal. By using single-crystal spectrophotometry, reactions taking place in the crystal can be monitored, either to trap intermediates or follow photoreduction during X-ray data collection. By using neutron crystallography, the positions of H atoms can be located, as it is the nuclei rather than the electrons that scatter neutrons, and the scattering length is not determined by the atomic number. Combining the two techniques allows much greater insight into both reaction mechanism and X-ray-induced photoreduction.

X-ray absorption spectroscopy: EXAFS (Extended X-ray Absorption Fine Structure) and XANES (X-ray Absorption Near Edge Structure)

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

Alp, E.E.; Mini, S.M.; Ramanathan, M.

1990-04-01

The x-ray absorption spectroscopy (XAS) had been an essential tool to gather spectroscopic information about atomic energy level structure in the early decades of this century. It has also played an important role in the discovery and systematization of rare-earth elements. The discovery of synchrotron radiation in 1952, and later the availability of broadly tunable synchrotron based x-ray sources have revitalized this technique since the 1970's. The correct interpretation of the oscillatory structure in the x-ray absorption cross-section above the absorption edge by Sayers et. al. has transformed XAS from a spectroscopic tool to a structural technique. EXAFS (Extended X-raymore » Absorption Fine Structure) yields information about the interatomic distances, near neighbor coordination numbers, and lattice dynamics. An excellent description of the principles and data analysis techniques of EXAFS is given by Teo. XANES (X-ray Absorption Near Edge Structure), on the other hand, gives information about the valence state, energy bandwidth and bond angles. Today, there are about 50 experimental stations in various synchrotrons around the world dedicated to collecting x-ray absorption data from the bulk and surfaces of solids and liquids. In this chapter, we will give the basic principles of XAS, explain the information content of essentially two different aspects of the absorption process leading to EXAFS and XANES, and discuss the source and samples limitations.« less

PREFACE: Exploring surfaces and buried interfaces of functional materials by advanced x-ray and neutron techniques Exploring surfaces and buried interfaces of functional materials by advanced x-ray and neutron techniques

NASA Astrophysics Data System (ADS)

Sakurai, Kenji

2010-12-01

This special issue is devoted to describing recent applications of x-ray and neutron scattering techniques to the exploration of surfaces and buried interfaces of various functional materials. Unlike many other surface-sensitive methods, these techniques do not require ultra high vacuum, and therefore, a variety of real and complicated surfaces fall within the scope of analysis. It must be particularly emphasized that the techniques are capable of seeing even buried function interfaces as well as the surface. Furthermore, the information, which ranges from the atomic to mesoscopic scale, is highly quantitative and reproducible. The non-destructive nature of the techniques is another important advantage of using x-rays and neutrons, when compared with other atomic-scale analyses. This ensures that the same specimen can be measured by other techniques. Such features are fairly attractive when exploring multilayered materials with nanostructures (dots, tubes, wires, etc), which are finding applications in electronic, magnetic, optical and other devices. The Japan Applied Physics Society has established a group to develop the research field of studying buried function interfaces with x-rays and neutrons. As the methods can be applied to almost all types of materials, from semiconductor and electronic devices to soft materials, participants have fairly different backgrounds but share a common interest in state-of-the-art x-ray and neutron techniques and sophisticated applications. A series of workshops has been organized almost every year since 2001. Some international interactions have been continued intensively, although the community is part of a Japanese society. This special issue does not report the proceedings of the recent workshop, although all the authors are in some way involved in the activities of the above society. Initially, we intended to collect quite long overview papers, including the authors' latest and most important original results, as well as updates on recent progress and global trends in the field. We planned to cover quite a wide area of surface and buried interface science with x-rays and neutrons. Following a great deal of discussion during the editing process, we have decided to change direction. As we intend to publish similar special issues on a frequent basis, we will not insist on editing this issue as systematic and complete collections of research. Many authors decided to write an ordinary research paper rather than an article including systematic accounts. Due to this change in policy, some authors declined to contribute, and the number of papers is now just 12. However, readers will find that the special issue gives an interesting collection of new original research in surface and buried interface studies with x-rays and neutrons. The 12 papers cover the following research topics: (1) polymer analysis by diffuse scattering; (2) discussion of the electrochemical solid--liquid interface by synchrotron x-ray diffraction; (3) analysis of capped nanodots by grazing incidence small-angle x-ray scattering (GISAXS); (4) discussion of the strain distribution in silicon by high-resolution x-ray diffraction; (5) study of mesoporous structures by a combination of x-ray reflectivity and GISAXS; (6) discussion of energy-dispersive x-ray reflectometry and its applications; (7) neutron reflectivity studies on hydrogen terminated silicon interface; (8) the fabrication and performance of a special mirror for water windows; (9) depth selective analysis by total-reflection x-ray diffraction; (10) nanoparticle thin films prepared by a gas deposition technique; (11) discussion of crystal truncation rod (CTR) scattering of semiconductor nanostructures; (12) magnetic structure analysis of thin films by polarized neutron reflectivity. While not discussed in the present special issue, x-ray and neutron techniques have made great progress. The most important steps forward have been in 2D/3D real-space imaging, and realtime measurement. Advances in such technologies are bringing with them new opportunities in surface and buried interface science. In the not too distant future, we will publish a special issue or a book detailing such progress. Exploring surfaces and buried interfaces of functional materials by advanced x-ray and neutron techniques contents Lateral uniformity in chemical composition along a buried reaction front in polymers using off-specular reflectivity Kristopher A Lavery, Vivek M Prabhu, Sushil Satija and Wen-li Wu Orientation dependence of Pd growth on Au electrode surfaces M Takahasi, K Tamura, J Mizuki, T Kondo and K Uosaki A grazing incidence small-angle x-ray scattering analysis on capped Ge nanodots in layer structures Hiroshi Okuda, Masayuki Kato, Keiji Kuno, Shojiro Ochiai, Noritaka Usami, Kazuo Nakajima and Osami Sakata High resolution grazing-incidence in-plane x-ray diffraction for measuring the strain of a Si thin layer Kazuhiko Omote X-ray analysis of mesoporous silica thin films templated by Brij58 surfactant S Fall, M Kulij and A Gibaud Review of the applications of x-ray refraction and the x-ray waveguide phenomenon to estimation of film structures Kouichi Hayashi Epitaxial growth of largely mismatched crystals on H-terminated Si(111) surfaces Hidehito Asaoka Novel TiO2/ZnO multilayer mirrors at 'water-window' wavelengths fabricated by atomic layer epitaxy H Kumagai, Y Tanaka, M Murata, Y Masuda and T Shinagawa Depth-selective structural analysis of thin films using total-external-reflection x-ray diffraction Tomoaki Kawamura and Hiroo Omi Structures of Yb nanoparticle thin films grown by deposition in He and N2 gas atmospheres: AFM and x-ray reflectivity studies Martin Jerab and Kenji Sakurai Ga and As composition profiles in InP/GaInAs/InP heterostructures—x-ray CTR scattering and cross-sectional STM measurements Yoshikazu Takeda, Masao Tabuchi and Arao Nakamura Polarized neutron reflectivity study of a thermally treated MnIr/CoFe exchange bias system Naoki Awaji, Toyoo Miyajima, Shuuichi Doi and Kenji Nomura

New two-dimensional space-resolving flux detection technique for measurement of hohlraum inner radiation in Shenguang-III prototype.

PubMed

Ren, Kuan; Liu, Shenye; Du, Huabing; Hou, Lifei; Jing, Longfei; Zhao, Yang; Yang, Zhiwen; Wei, Minxi; Deng, Keli; Yao, Li; Yang, Guohong; Li, Sanwei; Lan, Ke; Liu, Jie; Zhu, Xiaoli; Ding, Yongkun; Yi, Lin

2015-10-01

The space-resolving measurement of X-ray flux from a specific area (laser spot, re-emitting wall, or capsule) inside the hohlraum is an ongoing and critical problem in indirectly driven inertial-confinement fusion experiments. In this work, we developed a new two-dimensional space-resolving flux detection technique to measure the X-ray flux from specific areas inside the hohlraum by using the time- and space-resolving flux detector (SRFD). In two typical hohlraum experiments conducted at the Shenguang-III prototype laser facility, the X-ray flux and radiation temperature from an area 0.2 mm in diameter inside the hohlraum were measured through the laser entrance hole (LEH). The different flux intensities and radiation temperatures detected using the SRFD from the inner area of the LEH were compared with the result measured using the flat-response X-ray detector from the entire LEH. This comparison was also analyzed theoretically. The inner area detected using the SRFD was found to be the re-emitting wall area alone. This important improvement in space-resolving X-ray flux measurement will enhance the current X-ray flux space characterization techniques, thereby furthering the quantitative understanding of X-ray flux space behavior in the hohlraum.

New two-dimensional space-resolving flux detection technique for measurement of hohlraum inner radiation in Shenguang-III prototype

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

Ren, Kuan; Research Center of Laser Fusion, China Academy of Engineering Physics, P.O. Box 919-986, Mianyang 621900; Liu, Shenye, E-mail: lsye1029@163.com

2015-10-15

The space-resolving measurement of X-ray flux from a specific area (laser spot, re-emitting wall, or capsule) inside the hohlraum is an ongoing and critical problem in indirectly driven inertial-confinement fusion experiments. In this work, we developed a new two-dimensional space-resolving flux detection technique to measure the X-ray flux from specific areas inside the hohlraum by using the time- and space-resolving flux detector (SRFD). In two typical hohlraum experiments conducted at the Shenguang-III prototype laser facility, the X-ray flux and radiation temperature from an area 0.2 mm in diameter inside the hohlraum were measured through the laser entrance hole (LEH). Themore » different flux intensities and radiation temperatures detected using the SRFD from the inner area of the LEH were compared with the result measured using the flat-response X-ray detector from the entire LEH. This comparison was also analyzed theoretically. The inner area detected using the SRFD was found to be the re-emitting wall area alone. This important improvement in space-resolving X-ray flux measurement will enhance the current X-ray flux space characterization techniques, thereby furthering the quantitative understanding of X-ray flux space behavior in the hohlraum.« less

From synchrotron radiation to lab source: advanced speckle-based X-ray imaging using abrasive paper

NASA Astrophysics Data System (ADS)

Wang, Hongchang; Kashyap, Yogesh; Sawhney, Kawal

2016-02-01

X-ray phase and dark-field imaging techniques provide complementary and inaccessible information compared to conventional X-ray absorption or visible light imaging. However, such methods typically require sophisticated experimental apparatus or X-ray beams with specific properties. Recently, an X-ray speckle-based technique has shown great potential for X-ray phase and dark-field imaging using a simple experimental arrangement. However, it still suffers from either poor resolution or the time consuming process of collecting a large number of images. To overcome these limitations, in this report we demonstrate that absorption, dark-field, phase contrast, and two orthogonal differential phase contrast images can simultaneously be generated by scanning a piece of abrasive paper in only one direction. We propose a novel theoretical approach to quantitatively extract the above five images by utilising the remarkable properties of speckles. Importantly, the technique has been extended from a synchrotron light source to utilise a lab-based microfocus X-ray source and flat panel detector. Removing the need to raster the optics in two directions significantly reduces the acquisition time and absorbed dose, which can be of vital importance for many biological samples. This new imaging method could potentially provide a breakthrough for numerous practical imaging applications in biomedical research and materials science.

Enhanced renal image contrast by ethanol fixation in phase-contrast X-ray computed tomography.

PubMed

Shirai, Ryota; Kunii, Takuya; Yoneyama, Akio; Ooizumi, Takahito; Maruyama, Hiroko; Lwin, Thet Thet; Hyodo, Kazuyuki; Takeda, Tohoru

2014-07-01

Phase-contrast X-ray imaging using a crystal X-ray interferometer can depict the fine structures of biological objects without the use of a contrast agent. To obtain higher image contrast, fixation techniques have been examined with 100% ethanol and the commonly used 10% formalin, since ethanol causes increased density differences against background due to its physical properties and greater dehydration of soft tissue. Histological comparison was also performed. A phase-contrast X-ray system was used, fitted with a two-crystal X-ray interferometer at 35 keV X-ray energy. Fine structures, including cortex, tubules in the medulla, and the vessels of ethanol-fixed kidney could be visualized more clearly than that of formalin-fixed tissues. In the optical microscopic images, shrinkage of soft tissue and decreased luminal space were observed in ethanol-fixed kidney; and this change was significantly shown in the cortex and outer stripe of the outer medulla. The ethanol fixation technique enhances image contrast by approximately 2.7-3.2 times in the cortex and the outer stripe of the outer medulla; the effect of shrinkage and the physical effect of ethanol cause an increment of approximately 78% and 22%, respectively. Thus, the ethanol-fixation technique enables the image contrast to be enhanced in phase-contrast X-ray imaging.

The BL LAC phenomenon: X-ray observations of transition objects and determination of the x-ray spectrum of a complete sample of flat-spectrum radio sources

NASA Technical Reports Server (NTRS)

Worrall, Diana M.

1994-01-01

This report summarizes the activities related to two ROSAT investigations: (1) x-ray properties of radio galaxies thought to contain BL Lac type nuclei; and (2) x-ray spectra of a complete sample of flat-spectrum radio sources. The following papers describing the research are provided as attachments: Multiple X-ray Emission Components in Low Power Radio Galaxies; New X-ray Results on Radio Galaxies; Analysis Techniques for a Multiwavelength Study of Radio Galaxies; Separation of X-ray Emission Components in Radio Galaxies; X-ray Emission in Powerful Radio Galaxies and Quasars; Extended and Compact X-ray Emission in Powerful Radio Galaxies; and X-ray Spectra of a Complete Sample of Extragalactic Core-dominated Radio Sources.

New developments of X-ray fluorescence imaging techniques in laboratory

NASA Astrophysics Data System (ADS)

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

2015-11-01

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

Digital enhancement of X-rays for NDT

NASA Technical Reports Server (NTRS)

Butterfield, R. L.

1980-01-01

Report is "cookbook" for digital processing of industrial X-rays. Computer techniques, previously used primarily in laboratory and developmental research, have been outlined and codified into step by step procedures for enhancing X-ray images. Those involved in nondestructive testing should find report valuable asset, particularly is visual inspection is method currently used to process X-ray images.

Selection of bioindicators to detect lead pollution in Ebro delta microbial mats, using high-resolution microscopic techniques.

PubMed

Maldonado, J; Solé, A; Puyen, Z M; Esteve, I

2011-07-01

Lead (Pb) is a metal that is non-essential to any metabolic process and, moreover, highly deleterious to life. In microbial mats - benthic stratified ecosystems - located in coastal areas, phototrophic microorganisms (algae and oxygenic phototrophic bacteria) are the primary producers and they are exposed to pollution by metals. In this paper we describe the search for bioindicators among phototrophic populations of Ebro delta microbial mats, using high-resolution microscopic techniques that we have optimized in previous studies. Confocal laser scanning microscopy coupled to a spectrofluorometric detector (CLSM-λscan) to determine in vivo sensitivity of different cyanobacteria to lead, and scanning electron microscopy (SEM) and transmission electron microscopy (TEM), both coupled to energy dispersive X-ray microanalysis (EDX), to determine the extra- and intracellular sequestration of this metal in cells, were the techniques used for this purpose. Oscillatoria sp. PCC 7515, Chroococcus sp. PCC 9106 and Spirulina sp. PCC 6313 tested in this paper could be considered bioindicators for lead pollution, because all of these microorganisms are indigenous, have high tolerance to high concentrations of lead and are able to accumulate this metal externally in extracellular polymeric substances (EPS) and intracellularly in polyphosphate (PP) inclusions. Experiments made with microcosms demonstrated that Phormidium-like and Lyngbya-like organisms selected themselves at the highest concentrations of lead assayed. In the present study it is shown that all cyanobacteria studied (both in culture and in microcosms) present PP inclusions in their cytoplasm and that these increase in number in lead polluted cultures and microcosms. We believe that the application of these microscopic techniques open up broad prospects for future studies of metal ecotoxicity. Copyright © 2011 Elsevier B.V. All rights reserved.

Dental Radiology I Student Guide [and Instructor Guide].

ERIC Educational Resources Information Center

Fox Valley Technical Coll., Appleton, WI.

The dental radiology student and instructor guides provide instruction in the following units: (1) x-ray physics; (2) x-ray production; (3) radiation health and safety; (4) radiographic anatomy and pathology; (5) darkroom setup and chemistry; (6) bisecting angle technique; (7) paralleling technique; (8) full mouth survey technique--composition and…

Distant Cluster Hunting. II; A Comparison of X-Ray and Optical Cluster Detection Techniques and Catalogs from the ROSAT Optical X-Ray Survey

NASA Technical Reports Server (NTRS)

Donahue, Megan; Scharf, Caleb A.; Mack, Jennifer; Lee, Y. Paul; Postman, Marc; Rosait, Piero; Dickinson, Mark; Voit, G. Mark; Stocke, John T.

2002-01-01

We present and analyze the optical and X-ray catalogs of moderate-redshift cluster candidates from the ROSA TOptical X-Ray Survey, or ROXS. The survey covers the sky area contained in the fields of view of 23 deep archival ROSA T PSPC pointings, 4.8 square degrees. The cross-correlated cluster catalogs were con- structed by comparing two independent catalogs extracted from the optical and X-ray bandpasses, using a matched-filter technique for the optical data and a wavelet technique for the X-ray data. We cross-identified cluster candidates in each catalog. As reported in Paper 1, the matched-filter technique found optical counter- parts for at least 60% (26 out of 43) of the X-ray cluster candidates; the estimated redshifts from the matched filter algorithm agree with at least 7 of 1 1 spectroscopic confirmations (Az 5 0.10). The matched filter technique. with an imaging sensitivity of ml N 23, identified approximately 3 times the number of candidates (155 candidates, 142 with a detection confidence >3 u) found in the X-ray survey of nearly the same area. There are 57 X-ray candidates, 43 of which are unobscured by scattered light or bright stars in the optical images. Twenty-six of these have fairly secure optical counterparts. We find that the matched filter algorithm, when applied to images with galaxy flux sensitivities of mI N 23, is fairly well-matched to discovering z 5 1 clusters detected by wavelets in ROSAT PSPC exposures of 8000-60,000 s. The difference in the spurious fractions between the optical and X-ray (30%) and IO%, respectively) cannot account for the difference in source number. In Paper I, we compared the optical and X-ray cluster luminosity functions and we found that the luminosity functions are consistent if the relationship between X-ray and optical luminosities is steep (Lx o( L&f). Here, in Paper 11, we present the cluster catalogs and a numerical simulation of the ROXS. We also present color-magnitude plots for several of the cluster candidates, and examine the prominence of the red sequence in each. We find that the X-ray clusters in our survey do not all have a prominent red sequence. We conclude that while the red sequence may be a distinct feature in the color-magnitude plots for virialized massive clusters, it may be less distinct in lower mass clusters of galaxies at even moderate redshifts. Multiple, complementary methods of selecting and defining clusters may be essential, particularly at high redshift where all methods start to run into completeness limits, incomplete understanding of physical evolution, and projection effects.

New X-Ray Technique to Characterize Nanoscale Precipitates in Aged Aluminum Alloys

NASA Astrophysics Data System (ADS)

Sitdikov, V. D.; Murashkin, M. Yu.; Valiev, R. Z.

2017-10-01

This paper puts forward a new technique for measurement of x-ray patterns, which enables to solve the problem of identification and determination of precipitates (nanoscale phases) in metallic alloys of the matrix type. The minimum detection limit of precipitates in the matrix of the base material provided by this technique constitutes as little as 1%. The identification of precipitates in x-ray patterns and their analysis are implemented through a transmission mode with a larger radiation area, longer holding time and higher diffractometer resolution as compared to the conventional reflection mode. The presented technique has been successfully employed to identify and quantitatively describe precipitates formed in the Al alloy of the Al-Mg-Si system as a result of artificial aging. For the first time, the x-ray phase analysis has been used to identify and measure precipitates formed during the alloy artificial aging.

Nondestructive Evaluation (NDE) for Inspection of Composite Sandwich Structures

NASA Technical Reports Server (NTRS)

Zalameda, Joseph N.; Parker, F. Raymond

2014-01-01

Composite honeycomb structures are widely used in aerospace applications due to their low weight and high strength advantages. Developing nondestructive evaluation (NDE) inspection methods are essential for their safe performance. Flash thermography is a commonly used technique for composite honeycomb structure inspections due to its large area and rapid inspection capability. Flash thermography is shown to be sensitive for detection of face sheet impact damage and face sheet to core disbond. Data processing techniques, using principal component analysis to improve the defect contrast, are discussed. Limitations to the thermal detection of the core are investigated. In addition to flash thermography, X-ray computed tomography is used. The aluminum honeycomb core provides excellent X-ray contrast compared to the composite face sheet. The X-ray CT technique was used to detect impact damage, core crushing, and skin to core disbonds. Additionally, the X-ray CT technique is used to validate the thermography results.

Bismuth Passivation Technique for High-Resolution X-Ray Detectors

NASA Technical Reports Server (NTRS)

Chervenak, James; Hess, Larry

2013-01-01

The Athena-plus team requires X-ray sensors with energy resolution of better than one part in 3,000 at 6 keV X-rays. While bismuth is an excellent material for high X-ray stopping power and low heat capacity (for large signal when an X-ray is stopped by the absorber), oxidation of the bismuth surface can lead to electron traps and other effects that degrade the energy resolution. Bismuth oxide reduction and nitride passivation techniques analogous to those used in indium passivation are being applied in a new technique. The technique will enable improved energy resolution and resistance to aging in bismuth-absorber-coupled X-ray sensors. Elemental bismuth is lithographically integrated into X-ray detector circuits. It encounters several steps where the Bi oxidizes. The technology discussed here will remove oxide from the surface of the Bi and replace it with nitridized surface. Removal of the native oxide and passivating to prevent the growth of the oxide will improve detector performance and insulate the detector against future degradation from oxide growth. Placing the Bi coated sensor in a vacuum system, a reduction chemistry in a plasma (nitrogen/hydrogen (N2/H2) + argon) is used to remove the oxide and promote nitridization of the cleaned Bi surface. Once passivated, the Bi will perform as a better X-ray thermalizer since energy will not be trapped in the bismuth oxides on the surface. A simple additional step, which can be added at various stages of the current fabrication process, can then be applied to encapsulate the Bi film. After plasma passivation, the Bi can be capped with a non-diffusive layer of metal or dielectric. A non-superconducting layer is required such as tungsten or tungsten nitride (WNx).

Laboratory-size three-dimensional water-window x-ray microscope with Wolter type I mirror optics

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

Ohsuka, Shinji; The Graduate School for the Creation of New Photonics Industries, 1955-1 Kurematsu-cho, Nishi-ku, Hamamatsu-City, 431-1202; Ohba, Akira

2016-01-28

We constructed a laboratory-size three-dimensional water-window x-ray microscope that combines wide-field transmission x-ray microscopy with tomographic reconstruction techniques. It consists of an electron-impact x-ray source emitting oxygen Kα x-rays, Wolter type I grazing incidence mirror optics, and a back-illuminated CCD for x-ray imaging. A spatial resolution limit better than 1.0 line pairs per micrometer was obtained for two-dimensional transmission images, and 1-μm-scale three-dimensional fine structures were resolved.

Phase-contrast x-ray computed tomography for observing biological specimens and organic materials

NASA Astrophysics Data System (ADS)

Momose, Atsushi; Takeda, Tohoru; Itai, Yuji

1995-02-01

A novel three-dimensional x-ray imaging method has been developed by combining a phase-contrast x-ray imaging technique with x-ray computed tomography. This phase-contrast x-ray computed tomography (PCX-CT) provides sectional images of organic specimens that would produce absorption-contrast x-ray CT images with little contrast. Comparing PCX-CT images of rat cerebellum and cancerous rabbit liver specimens with corresponding absorption-contrast CT images shows that PCX-CT is much more sensitive to the internal structure of organic specimens.

Practical application of cross correlation technique to measure jitter of master-oscillator-power-amplifier laser system

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

Młyńczak, J.; Sawicz-Kryniger, K.; Fry, A. R.

2014-01-01

The Linac coherent light source (LCLS) at the SLAC National Accelerator Laboratory (SLAC) is the world’s first hard X-ray free electron laser (XFEL) and is capable of producing high-energy, femtosecond duration X-ray pulses. A common technique to study fast timescale physical phenomena, various “pump/probe” techniques are used. In these techniques there are two lasers, one optical and one X-ray, that work as a pump and as a probe to study dynamic processes in atoms and molecules. In order to resolve phenomena that occur on femtosecond timescales, it is imperative to have very precise timing between the optical lasers and X-raysmore » (on the order of ~ 20 fs or better). The lasers are synchronized to the same RF source that drives the accelerator and produces the X-ray laser. However, elements in the lasers cause some drift and time jitter, thereby de-synchronizing the system. This paper considers cross-correlation technique as a way to quantify the drift and jitter caused by the regenerative amplifier of the ultrafast optical laser.« less

Toward in situ x-ray diffraction imaging at the nanometer scale

NASA Astrophysics Data System (ADS)

Zatsepin, Nadia A.; Dilanian, Ruben A.; Nikulin, Andrei Y.; Gable, Brian M.; Muddle, Barry C.; Sakata, Osami

2008-08-01

We present the results of preliminary investigations determining the sensitivity and applicability of a novel x-ray diffraction based nanoscale imaging technique, including simulations and experiments. The ultimate aim of this nascent technique is non-destructive, bulk-material characterization on the nanometer scale, involving three dimensional image reconstructions of embedded nanoparticles and in situ sample characterization. The approach is insensitive to x-ray coherence, making it applicable to synchrotron and laboratory hard x-ray sources, opening the possibility of unprecedented nanometer resolution with the latter. The technique is being developed with a focus on analyzing a technologically important light metal alloy, Al-xCu (where x is 2.0-5.0 %wt). The mono- and polycrystalline samples contain crystallographically oriented, weakly diffracting Al2Cu nanoprecipitates in a sparse, spatially random dispersion within the Al matrix. By employing a triple-axis diffractometer in the non-dispersive setup we collected two-dimensional reciprocal space maps of synchrotron x-rays diffracted from the Al2Cu nanoparticles. The intensity profiles of the diffraction peaks confirmed the sensitivity of the technique to the presence and orientation of the nanoparticles. This is a fundamental step towards in situ observation of such extremely sparse, weakly diffracting nanoprecipitates embedded in light metal alloys at early stages of their growth.

A three-image algorithm for hard x-ray grating interferometry.

PubMed

Pelliccia, Daniele; Rigon, Luigi; Arfelli, Fulvia; Menk, Ralf-Hendrik; Bukreeva, Inna; Cedola, Alessia

2013-08-12

A three-image method to extract absorption, refraction and scattering information for hard x-ray grating interferometry is presented. The method comprises a post-processing approach alternative to the conventional phase stepping procedure and is inspired by a similar three-image technique developed for analyzer-based x-ray imaging. Results obtained with this algorithm are quantitatively comparable with phase-stepping. This method can be further extended to samples with negligible scattering, where only two images are needed to separate absorption and refraction signal. Thanks to the limited number of images required, this technique is a viable route to bio-compatible imaging with x-ray grating interferometer. In addition our method elucidates and strengthens the formal and practical analogies between grating interferometry and the (non-interferometric) diffraction enhanced imaging technique.

The relationship between wave and geometrical optics models of coded aperture type x-ray phase contrast imaging systems

PubMed Central

Munro, Peter R.T.; Ignatyev, Konstantin; Speller, Robert D.; Olivo, Alessandro

2013-01-01

X-ray phase contrast imaging is a very promising technique which may lead to significant advancements in medical imaging. One of the impediments to the clinical implementation of the technique is the general requirement to have an x-ray source of high coherence. The radiation physics group at UCL is currently developing an x-ray phase contrast imaging technique which works with laboratory x-ray sources. Validation of the system requires extensive modelling of relatively large samples of tissue. To aid this, we have undertaken a study of when geometrical optics may be employed to model the system in order to avoid the need to perform a computationally expensive wave optics calculation. In this paper, we derive the relationship between the geometrical and wave optics model for our system imaging an infinite cylinder. From this model we are able to draw conclusions regarding the general applicability of the geometrical optics approximation. PMID:20389424

The relationship between wave and geometrical optics models of coded aperture type x-ray phase contrast imaging systems.

PubMed

Munro, Peter R T; Ignatyev, Konstantin; Speller, Robert D; Olivo, Alessandro

2010-03-01

X-ray phase contrast imaging is a very promising technique which may lead to significant advancements in medical imaging. One of the impediments to the clinical implementation of the technique is the general requirement to have an x-ray source of high coherence. The radiation physics group at UCL is currently developing an x-ray phase contrast imaging technique which works with laboratory x-ray sources. Validation of the system requires extensive modelling of relatively large samples of tissue. To aid this, we have undertaken a study of when geometrical optics may be employed to model the system in order to avoid the need to perform a computationally expensive wave optics calculation. In this paper, we derive the relationship between the geometrical and wave optics model for our system imaging an infinite cylinder. From this model we are able to draw conclusions regarding the general applicability of the geometrical optics approximation.

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

NASA Technical Reports Server (NTRS)

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

1993-01-01

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

Synchrotron x-ray imaging of acoustic cavitation bubbles induced by acoustic excitation

NASA Astrophysics Data System (ADS)

Jung, Sung Yong; Park, Han Wook; Park, Sung Ho; Lee, Sang Joon

2017-04-01

The cavitation induced by acoustic excitation has been widely applied in various biomedical applications because cavitation bubbles can enhance the exchanges of mass and energy. In order to minimize the hazardous effects of the induced cavitation, it is essential to understand the spatial distribution of cavitation bubbles. The spatial distribution of cavitation bubbles visualized by the synchrotron x-ray imaging technique is compared to that obtained with a conventional x-ray tube. Cavitation bubbles with high density in the region close to the tip of the probe are visualized using the synchrotron x-ray imaging technique, however, the spatial distribution of cavitation bubbles in the whole ultrasound field is not detected. In this study, the effects of the ultrasound power of acoustic excitation and working medium on the shape and density of the induced cavitation bubbles are examined. As a result, the synchrotron x-ray imaging technique is useful for visualizing spatial distributions of cavitation bubbles, and it could be used for optimizing the operation conditions of acoustic cavitation.

Cobalt distribution in keratinocyte cells indicates nuclear and perinuclear accumulation and interaction with magnesium and zinc homeostasis.

PubMed

Ortega, Richard; Bresson, Carole; Fraysse, Aurélien; Sandre, Caroline; Devès, Guillaume; Gombert, Clémentine; Tabarant, Michel; Bleuet, Pierre; Seznec, Hervé; Simionovici, Alexandre; Moretto, Philippe; Moulin, Christophe

2009-07-10

Cobalt is known to be toxic at high concentration, to induce contact dermatosis, and occupational radiation skin damage because of its use in nuclear industry. We investigated the intracellular distribution of cobalt in HaCaT human keratinocytes as a model of skin cells, and its interaction with endogenous trace elements. Direct micro-chemical imaging based on ion beam techniques was applied to determine the quantitative distribution of cobalt in HaCaT cells. In addition, synchrotron radiation X-ray fluorescence microanalysis in tomography mode was performed, for the first time on a single cell, to determine the 3D intracellular distribution of cobalt. Results obtained with these micro-chemical techniques were compared to a more classical method based on cellular fractionation followed by inductively coupled plasma atomic emission spectrometry (ICP-AES) measurements. Cobalt was found to accumulate in the cell nucleus and in perinuclear structures indicating the possible direct interaction with genomic DNA, and nuclear proteins. The perinuclear accumulation in the cytosol suggests that cobalt could be stored in the endoplasmic reticulum or the Golgi apparatus. The multi-elemental analysis revealed that cobalt exposure significantly decreased magnesium and zinc content, with a likely competition of cobalt for magnesium and zinc binding sites in proteins. Overall, these data suggest a multiform toxicity of cobalt related to interactions with genomic DNA and nuclear proteins, and to the alteration of zinc and magnesium homeostasis.

New electrocatalysts for unitized regenerative fuel cell: Pt-Ir alloy deposited on the proton exchange membrane surface by impregnation-reduction method.

PubMed

Wan, Chieh-Hao; Wu, Chun-Lin; Lin, Meng-Tsun; Shih, Chihhsiong

2010-07-01

In this paper, a modified technique to prepare Pt-Ir catalyst layer on the proton exchange membrane (PEM) surface using the impregnation-reduction (IR) method is proposed to improve the electrocatalytic activity as well as the life cycle of the bifunctional oxygen electrode (BOE). The resulted electrocatalysts were characterized by the Scanning Electron Microscopy (SEM), X-ray Diffraction (XRD), Electron Probe Micro-Analysis (EPMA), and Transmission Electron Microscope (TEM). The electrocatalytic properties of the Pt-Ir layer on PEM surface for the oxygen reduction and water oxidation reactions as well as the life cycle of MEA were investigated. Experimental results showed that the Ir particles were dispersed densely in the platinum layer through the modified IR technique. The atomic ratio of Pt over Ir elements was 9:1, and the resulted thickness of the obtained Pt-Ir catalyst layer was about 1.0 microm. The Pt-Ir catalyst layer was composed of Pt layer doped with Ir nano-particles comprising nano Pt-Ir alloy phase. The large surface area of Ir core with Pt shell particles and the presence of nano Pt-Ir alloy phase led to a higher electrocatalytic activity of BOE. Due to the good binding between the Nafion membrane and the Pt-Ir alloy catalyst, as well as the composite structure of the resulted Pt-Ir, the life cycle of Unitized Regenerative Fuel Cell (URFC) is improved through this novel BOE.

Spectra of cosmic X-ray sources

NASA Technical Reports Server (NTRS)

Holt, S. S.; Mccray, R.

1982-01-01

X-ray measurements provide the most direct probes of astrophysical environments with temperatures exceeding one million K. Progress in experimental research utilizing dispersive techniques (e.g., Bragg and grating spectroscopy) is considerably slower than that in areas utilizing photometric techniques, because of the relative inefficiency of the former for the weak X-ray signals from celestial sources. As a result, the term "spectroscopy" as applied to X-ray astronomy has traditionally satisfied a much less restrictive definition (in terms of resolving power) than it has in other wavebands. Until quite recently, resolving powers of order unity were perfectly respectable, and still provide (in most cases) the most useful spectroscopic data. In the broadest sense, X-ray photometric measurements are spectroscopic, insofar as they represent samples of the overall electromagnetic continua of celestial objects.

Simultaneous parameter optimization of x-ray and neutron reflectivity data using genetic algorithms

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

Singh, Surendra, E-mail: surendra@barc.gov.in; Basu, Saibal

2016-05-23

X-ray and neutron reflectivity are two non destructive techniques which provide a wealth of information on thickness, structure and interracial properties in nanometer length scale. Combination of X-ray and neutron reflectivity is well suited for obtaining physical parameters of nanostructured thin films and superlattices. Neutrons provide a different contrast between the elements than X-rays and are also sensitive to the magnetization depth profile in thin films and superlattices. The real space information is extracted by fitting a model for the structure of the thin film sample in reflectometry experiments. We have applied a Genetic Algorithms technique to extract depth dependentmore » structure and magnetic in thin film and multilayer systems by simultaneously fitting X-ray and neutron reflectivity data.« less

Spectroscopic imaging, diffraction, and holography with x-ray photoemission

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

Not Available

1992-02-01

X-ray probes are capable of determining the spatial structure of an atom in a specific chemical state, over length scales from about a micron all the way down to atomic resolution. Examples of these probes include photoemission microscopy, energy-dependent photoemission diffraction, photoelectron holography, and X-ray absorption microspectroscopy. Although the method of image formation, chemical-state sensitivity, and length scales can be very different, these X-ray techniques share a common goal of combining a capability for structure determination with chemical-state specificity. This workshop will address recent advances in holographic, diffraction, and direct imaging techniques using X-ray photoemission on both theoretical and experimentalmore » fronts. A particular emphasis will be on novel structure determinations with atomic resolution using photoelectrons.« less

Using acoustic levitation in synchrotron based laser pump hard x-ray probe experiments

NASA Astrophysics Data System (ADS)

Hu, Bin; Lerch, Jason; Suthar, Kamlesh; Dichiara, Anthony

Acoustic levitation provides a platform to trap and hold a small amount of material by using standing pressure waves without a container. The technique has a potential to be used for laser pump x-ray probe experiments; x-ray scattering and laser distortion from the container can be avoided, sample consumption can be minimized, and unwanted chemistry that may occur at the container interface can be avoided. The method has been used at synchrotron sources for studying protein and pharmaceutical solutions using x-ray diffraction (XRD) and small angle x-ray scattering (SAXS). However, pump-probe experiments require homogeneously excited samples, smaller than the absorption depth of the material that must be held stably at the intersection of both the laser and x-ray beams. We discuss 1) the role of oscillations in acoustic levitation and the optimal acoustic trapping conditions for x-ray/laser experiments, 2) opportunities to automate acoustic levitation for fast sample loading and manipulation, and 3) our experimental results using SAXS to monitor laser induced thermal expansion in gold nanoparticles solution. We also performed Finite Element Analysis to optimize the trapping performance and stability of droplets ranging from 0.4 mm to 2 mm. Our early x-ray/laser demonstrated the potential of the technique for time-resolved X-ray science.

Ultrastructure, Histochemistry, and Mineralization Patterns in the Ecdysial Suture of the Blue Crab, Callinectes sapidus

NASA Astrophysics Data System (ADS)

Priester, Carolina; Dillaman, Richard M.; Gay, D. Mark

2005-12-01

The ecdysial suture is the region of the arthropod exoskeleton that splits to allow the animal to emerge during ecdysis. We examined the morphology and composition of the intermolt and premolt suture of the blue crab using light microscopy and scanning electron microscopy. The suture could not be identified by routine histological techniques; however 3 of 22 fluorescein isothiocyanate-labeled lectins tested (Lens culinaris agglutinin, Vicia faba agglutinin, and Pisum sativum agglutinin) differentiated the suture, binding more intensely to the suture exocuticle and less intensely to the suture endocuticle. Back-scattered electron (BSE) and secondary electron observations of fracture surfaces of intermolt cuticle showed less mineralized regions in the wedge-shaped suture as did BSE analysis of premolt and intermolt resin-embedded cuticle. The prism regions of the suture exocuticle were not calcified. X-ray microanalysis of both the endocuticle and exocuticle demonstrated that the suture was less calcified than the surrounding cuticle with significantly lower magnesium and phosphorus concentrations, potentially making its mineral more soluble. The presence or absence of a glycoprotein in the organic matrix, the extent and composition of the mineral deposited, and the thickness of the cuticle all likely contribute to the suture being removed by molting fluid, thereby ensuring successful ecdysis.

Influence of nitrogen in the shielding gas on corrosion resistance of duplex stainless steel welds

NASA Astrophysics Data System (ADS)

Bhatt, R. B.; Kamat, H. S.; Ghosal, S. K.; de, P. K.

1999-10-01

The influence of nitrogen in shielding gas on the corrosion resistance of welds of a duplex stainless steel (grade U-50), obtained by gas tungsten arc (GTA) with filler wire, autogenous GTA (bead-on-plate), electron beam welding (EBW), and microplasma techniques, has been evaluated in chloride solutions at 30 °C. Pitting attack has been observed in GTA, electron beam welding, and microplasma welds when welding has been carried out using pure argon as the shielding gas. Gas tungsten arc welding with 5 to 10% nitrogen and 90 to 95% argon, as the shielding gas, has been found to result in an improved pitting corrosion resistance of the weldments of this steel. However, the resistance to pitting of autogenous welds (bead-on-plate) obtained in pure argon as the shielding gas has been observed to remain unaffected. Microscopic examination, electron probe microanalysis (EPMA), and x-ray diffraction studies have revealed that the presence of nitrogen in the shielding gas in the GTA welds not only modifies the microstructure and the austenite to ferrite ratio but also results in a nearly uniform distribution of the various alloying elements, for example, chromium, nickel, and molybdenum among the constitutent phases, which are responsible for improved resistance to pitting corrosion.

Effects of thermal treatments on microstructure and mechanical properties of a Co-Cr-Mo-W biomedical alloy produced by laser sintering.

PubMed

Mengucci, P; Barucca, G; Gatto, A; Bassoli, E; Denti, L; Fiori, F; Girardin, E; Bastianoni, P; Rutkowski, B; Czyrska-Filemonowicz, A

2016-07-01

Direct Metal Laser Sintering (DMLS) technology based on a layer by layer production process was used to produce a Co-Cr-Mo-W alloy specifically developed for biomedical applications. The alloy mechanical response and microstructure were investigated in the as-sintered state and after post-production thermal treatments. Roughness and hardness measurements, and tensile and flexural tests were performed to study the mechanical response of the alloy while X-ray diffraction (XRD), electron microscopy (SEM, TEM, STEM) techniques and microanalysis (EDX) were used to investigate the microstructure in different conditions. Results showed an intricate network of ε-Co (hcp) lamellae in the γ-Co (fcc) matrix responsible of the high UTS and hardness values in the as-sintered state. Thermal treatments increase volume fraction of the ε-Co (hcp) martensite but slightly modify the average size of the lamellar structure. Nevertheless, thermal treatments are capable of producing a sensible increase in UTS and hardness and a strong reduction in ductility. These latter effects were mainly attributed to the massive precipitation of an hcp Co3(Mo,W)2Si phase and the contemporary formation of Si-rich inclusions. Copyright © 2016 Elsevier Ltd. All rights reserved.

Sensitive, selective, disposable electrochemical dopamine sensor based on PEDOT-modified laser scribed graphene.

PubMed

Xu, Guangyuan; Jarjes, Zahraa A; Desprez, Valentin; Kilmartin, Paul A; Travas-Sejdic, Jadranka

2018-06-01

The fabrication of a novel, and highly selective electrochemical sensor based on a poly(3,4-ethylenedioxythiophene) (PEDOT) modified laser scribed graphene (LSG), and detection of dopamine (DA) in the presence of ascorbic acid (AA) and uric acid (UA) is described. LSG electrodes were produced with a 3-dimensional macro-porous network and large electrochemically-active surface area via direct laser writing on polyimide sheets. PEDOT was electrodeposited on the LSG electrode, and the physical properties of the obtained films were characterized by scanning electron microscopy (SEM) and energy dispersive X-ray diffraction microanalysis (EDAX). The modified electrodes were applied for the determination of DA in the presence of AA and UA using cyclic voltammetry (CV), and differential pulse voltammetry (DPV) techniques. The linear range for dopamine detection was found to be 1-150 µM with a sensitivity of 0.220 ± 0.011 µA μM -1 and a detection limit of 0.33 µM; superior values to those obtained without PEDOT. For the first time, PEDOT-modified LSG have been fabricated and assessed for high-performance dopamine sensing using cost-effective, disposable electrodes, with potential for development in further sensing applications. Copyright © 2018 Elsevier B.V. All rights reserved.

Mechanism and control of fluid secretion.

PubMed

Oschman, J L

1977-01-01

Fluid secretion and reabsorption by a variety of plant and animal tissues appear to be accomplished by osmotic coupling between solute transport and water movement. The local osmosis model suggests that active accumulation of solutes within narrow folds at the cell surface may produce the local gradients that generate water flow. Both micropuncture techniques and electron-probe X-ray microanalysis have established that local osmotic gradients occur in absorptive epithelia, but they have not as yet been detected in secretory tissues.Hormonal control of secretion involves stimulation of solute pumps and adjustments of permeability to non-transported solutes. Since hormone receptors and pumps are often located on opposite surfaces of the cell, intracellular second messengers convey the secretory signal through cytoplasm. Much has been learned by study of insect tissues that are anatomically simple and that function for long periods in vitro. Aspects of hormone-receptor interaction have been explored, including the action of halluninogenic molecules. In insect salivary glands cyclic AMP appears to stimulate cation transport, while calcium increases anion permeability. The various second messengers probably interact with each other in complex feedback loops that stabilize the system and make it quickly responsive to hormone. Cyclic AMP may stimulate release of calcium from mitochondria. Unresolved is the way second messengers alter properties of the cell surface.

Confocal laser scanning microscopy coupled to a spectrofluorometric detector as a rapid tool for determining the in vivo effect of metals on phototrophic bacteria.

PubMed

Burnat, Mireia; Diestra, Elia; Esteve, Isabel; Solé, Antonio

2010-01-01

In this paper, we determine for the first time the in vivo effect of heavy metals in a phototrophic bacterium. We used Confocal Laser Scanning Microscopy coupled to a spectrofluorometric detector as a rapid technique to measure pigment response to heavy-metal exposure. To this end, we selected lead and copper (toxic and essential metals) and Microcoleus sp. as the phototrophic bacterium because it would be feasible to see this cyanobacterium as a good biomarker, since it covers large extensions of coastal sediments. The results obtained demonstrate that, while cells are still viable, pigment peak decreases whereas metal concentration increases (from 0.1 to 1 mM Pb). Pigments are totally degraded when cultures were polluted with lead and copper at the maximum doses used (25 mM Pb(NO(3))(2) and 10 mM CuSO(4)). The aim of this study was also to identify the place of metal accumulation in Microcoleus cells. Element analysis of this cyanobacterium in the above mentioned conditions determined by Energy Dispersive X-ray microanalysis (EDX) coupled to Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM), shows that Pb (but not Cu) accumulates externally and internally in cells.

Influence of nitrogen in the shielding gas on corrosion resistance of duplex stainless steel welds

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

Bhatt, R.B.; Kamat, H.S.; Ghosal, S.K.

1999-10-01

The influence of nitrogen in shielding gas on the corrosion resistance of welds of a duplex stainless steel (grade U-50), obtained by gas tungsten arc (GTA) with filler wire, autogenous GTA (bead-on-plate), electron beam welding (EBW), and microplasma techniques, has been evaluated in chloride solutions at 30 C. Pitting attack has been observed in GTA, electron beam welding, and microplasma welds when welding has been carried out using pure argon as the shielding gas. Gas tungsten arc welding with 5 to 10% nitrogen and 90 to 95% argon, as the shielding gas, has been found to result in an improvedmore » pitting corrosion resistance of the weldments of this steel. However, the resistance of pitting of autogenous welds (bead-on-plate) obtained in pure argon as the shielding gas has been observed to remain unaffected. Microscopic examination, electron probe microanalysis (EPMA), and x-ray diffraction studies have revealed that the presence of nitrogen in the shielding gas in the GTA welds not only modifies the microstructure and the austenite to ferrite ratio but also results in a nearly uniform distribution of the various alloying elements, for example, chromium, nickel, and molybdenum among the constituent phases, which are responsible for improved resistance to pitting corrosion.« less

Microstructural analysis of laser weld fusion zone in Haynes 282 superalloy

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

Osoba, L.O.; Ding, R.G.; Ojo, O.A., E-mail: ojo@cc.umanitoba.ca

Analytical electron microscopy and spectroscopy analyses of the fusion zone (FZ) microstructure in autogenous laser beam welded Haynes 282 (HY 282) superalloy were performed. The micro-segregation patterns observed in the FZ indicate that Co, Cr and Al exhibited a nearly uniform distribution between the dendrite core and interdendritic regions while Ti and Mo were rejected into the interdendritic liquid during the weld solidification. Transmission electron diffraction analysis and energy dispersive X-ray microanalysis revealed the second phase particles formed along the FZ interdendritic region to be Ti-Mo rich MC-type carbide particles. Weld FZ solidification cracking, which is sometimes associated with themore » formation of {gamma}-{gamma}' eutectic in {gamma}' precipitation strengthened nickel-base superalloys, was not observed in the HY 282 superalloy. Modified primary solidification path due to carbon addition in the newly developed superalloy is used to explain preclusion of weld FZ solidification cracking in the material. - Highlights: Black-Right-Pointing-Pointer A newly developed superalloy was welded by CO{sub 2} laser beam joining technique. Black-Right-Pointing-Pointer Electron microscopy characterization of the weld microstructure was performed. Black-Right-Pointing-Pointer Identified interdendritic microconstituents consist of MC-type carbides. Black-Right-Pointing-Pointer Modification of primary solidification path is used to explain cracking resistance.« less

High-pressure-assisted X-ray-induced damage as a new route for materials synthesis

DOE PAGES

Evlyukhin, Egor; Kim, Eunja; Goldberger, David; ...

2018-01-01

X-ray radiation induced damage has been known for decades and has largely been viewed as a tremendous nuisance; e.g., most X-ray-related studies of organic and inorganic materials suffer X-ray damage to varying degrees. Although, recent theoretical and experimental investigation of the response of simple chemical systems to X-rays offered better understanding of the mechanistic details of X-ray induced damage, the question about useful applicability of this technique is still unclear. Furthermore we experimentally demonstrate that by tuning pressure and X-ray energy, the radiation induced damage can be controlled and used for synthesis of novel materials.

X-ray Spectrometry.

ERIC Educational Resources Information Center

Markowicz, Andrzej A.; Van Grieken, Rene E.

1984-01-01

Provided is a selective literature survey of X-ray spectrometry from late 1981 to late 1983. Literature examined focuses on: excitation (photon and electron excitation and particle-induced X-ray emission; detection (wavelength-dispersive and energy-dispersive spectrometry); instrumentation and techniques; and on such quantitative analytical…

Chemical imaging analysis of the brain with X-ray methods

NASA Astrophysics Data System (ADS)

Collingwood, Joanna F.; Adams, Freddy

2017-04-01

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

Analysis of photographic X-ray images. [S-054 telescope on Skylab

NASA Technical Reports Server (NTRS)

Krieger, A. S.

1977-01-01

Some techniques used to extract quantitative data from the information contained in photographic images produced by grazing incidence soft X-ray optical systems are described. The discussion is focussed on the analysis of the data returned by the S-054 X-Ray Spectrographic Telescope Experiment on Skylab. The parameters of the instrument and the procedures used for its calibration are described. The technique used to convert photographic density to focal plane X-ray irradiance is outlined. The deconvolution of the telescope point response function from the image data is discussed. Methods of estimating the temperature, pressure, and number density of coronal plasmas are outlined.

Elemental X-ray mapping of agglutinated foraminifer tests: A non- destructive technique for determining compositional characteristics.

USGS Publications Warehouse

Commeau, R.F.; Reynolds, Leslie A.; Poag, C.W.

1985-01-01

The composition of agglutinated foraminiferal tests vary remarkably in response to local substrate characteristics, physiochemical properties of the water column and species- dependant selectivity of test components. We have employed a technique that combines a scanning electron microscope with an energy dispersive X-ray spectrometer system to identify major and minor elemental constituents of agglutinated foraminiferal walls. As a sample is bombarded with a beam of high energy electrons, X-rays are generated that are characteristic of the elements present. As a result, X- ray density maps can be produced for each of several elements present in the tests of agglutinated foraminifers. 

Very high resolution UV and X-ray spectroscopy and imagery of solar active regions

NASA Technical Reports Server (NTRS)

Bruner, M.; Brown, W. A.; Haisch, B. M.

1987-01-01

A scientific investigation of the physics of the solar atmosphere, which uses the techniques of high resolution soft X-ray spectroscopy and high resolution UV imagery, is described. The experiments were conducted during a series of three sounding rocket flights. All three flights yielded excellent images in the UV range, showing unprecedented spatial resolution. The second flight recorded the X-ray spectrum of a solar flare, and the third that of an active region. A normal incidence multi-layer mirror was used during the third flight to make the first astronomical X-ray observations using this new technique.

High Resolution X-Ray Diffraction of Macromolecules with Synchrotron Radiation

NASA Technical Reports Server (NTRS)

Stojanoff, Vivian; Boggon, Titus; Helliwell, John R.; Judge, Russell; Olczak, Alex; Snell, Edward H.; Siddons, D. Peter; Rose, M. Franklin (Technical Monitor)

2000-01-01

We recently combined synchrotron-based monochromatic X-ray diffraction topography methods with triple axis diffractometry and rocking curve measurements: high resolution X-ray diffraction imaging techniques, to better understand the quality of protein crystals. We discuss these methods in the light of results obtained on crystals grown under different conditions. These non destructive techniques are powerful tools in the characterization of the protein crystals and ultimately will allow to improve, develop, and understand protein crystal growth. High resolution X-ray diffraction imaging methods will be discussed in detail in light of recent results obtained on Hen Egg White Lysozyme crystals and other proteins.

Echo-Enabled X-Ray Vortex Generation

NASA Astrophysics Data System (ADS)

Hemsing, E.; Marinelli, A.

2012-11-01

A technique to generate high-brightness electromagnetic vortices with tunable topological charge at extreme ultraviolet and x-ray wavelengths is described. Based on a modified version of echo-enabled harmonic generation for free-electron lasers, the technique uses two lasers and two chicanes to produce high-harmonic microbunching of a relativistic electron beam with a corkscrew distribution that matches the instantaneous helical phase structure of the x-ray vortex. The strongly correlated electron distribution emerges from an efficient three-dimensional recoherence effect in the echo-enabled harmonic generation transport line and can emit fully coherent vortices in a downstream radiator for access to new research in x-ray science.