Mars Microprobe Entry Analysis

NASA Technical Reports Server (NTRS)

Braun, Robert D.; Mitcheltree, Robert A.; Cheatwood, F. McNeil

1998-01-01

The Mars Microprobe mission will provide the first opportunity for subsurface measurements, including water detection, near the south pole of Mars. In this paper, performance of the Microprobe aeroshell design is evaluated through development of a six-degree-of-freedom (6-DOF) aerodynamic database and flight dynamics simulation. Numerous mission uncertainties are quantified and a Monte-Carlo analysis is performed to statistically assess mission performance. Results from this 6-DOF Monte-Carlo simulation demonstrate that, in a majority of the cases (approximately 2-sigma), the penetrator impact conditions are within current design tolerances. Several trajectories are identified in which the current set of impact requirements are not satisfied. From these cases, critical design parameters are highlighted and additional system requirements are suggested. In particular, a relatively large angle-of-attack range near peak heating is identified.

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.

PROTON MICROPROBE ANALYSIS OF TRACE-ELEMENT VARIATIONS IN VITRINITES IN THE SAME AND DIFFERENT COAL BEDS.

USGS Publications Warehouse

Minkin, J.A.; Chao, E.C.T.; Blank, Herma; Dulong, F.T.

1987-01-01

The PIXE (proton-induced X-ray emission) microprobe can be used for nondestructive, in-situ analyses of areas as small as those analyzed by the electron microprobe, and has a sensitivity of detection as much as two orders of magnitude better than the electron microprobe. Preliminary studies demonstrated that PIXE provides a capability for quantitative determination of elemental concentrations in individual coal maceral grains with a detection limit of 1-10 ppm for most elements analyzed. Encouraged by the earlier results, we carried out the analyses reported below to examine trace element variations laterally (over a km range) as well as vertically (cm to m) in the I and J coal beds in the Upper Cretaceous Ferron Sandstone Member of the Mancos Shale in central Utah, and to compare the data with the data from two samples of eastern coals of Pennsylvanian age.

Ion microprobe, electron microprobe and cathodoluminescence data for Allende inclusions with emphasis on plagioclase chemistry

NASA Technical Reports Server (NTRS)

Hutcheon, I. D.; Steele, I. M.; Smith, J. V.; Clayton, R. N.

1978-01-01

Three Type B inclusions from the Allende meteorite have been analyzed. A grain-to-grain characterization of mineral chemistry and isotopic content was made possible by the use of a range of techniques, including luminescence and scanning electron microscopy and electron and ion microprobe analysis. Cathodoluminescence was used in fine-grained, optically opaque regions to distinguish between sub-micrometer phases, such as garnet and Si-rich material, subsequently identified by electron probe and scanning electron microscope analyses. Four types of luminescence patterns, due to twinning, primary sector zoning, alteration of boundaries and fractures, and shock effects, were identified in Allende plagioclase. Luminescence color exhibited a strong correlation with Mg content and provided a guide for an electron probe quantitative map of Mg and Na distributions. Ion microprobe studies of individual grains revealed large excesses of Mg-26.

New Capabilities in the Analysis of Sub-micrometer Regions in Geological Materials with the Field Emission Electron Microprobe

NASA Astrophysics Data System (ADS)

Armstrong, J. T.; McSwiggen, P.; Nielsen, C.

2013-12-01

Quantitative electron microprobe analysis has revolutionized two-dimensional elemental analysis of Earth materials at the micrometer-scale. Newly available commercial field emission (FE-) source instruments represent significant technological advances in quantitative measurement with high spatial resolution at sub-micrometer scale - helping to bridge the gap between conventional microprobe and AEM analyses. Their performance specifications suggest the ability to extend routine quantitative analyses from ~3-5 micrometer diameter areas down to 1-2 micrometer diameter at beam energies of 15 keV; and, with care, down to 200-500 nm diameter at reduced beam energies. . In order to determine whether the level of performance suggested by the specifications is realistic, we spent a week doing analyses at the newly installed JEOL JXA-8530F field emission microprobe at Arizona State University, using a series of samples that are currently being studied in various projects at CIW. These samples included: 1) high-pressure experiment run product containing intergrowths of sub-micrometer grains of metal, sulfide, Fe-Mg-perovskite, and ferropericlase; 2) a thin section of the Ivankinsky basalt, part of the Siberian flood basalt sequence containing complex sub-micrometer intergrowths of magnetite, titanomagnetite, ilmenite, titanite and rutile; 3) a polished section of the Giroux pallasite, being studied for element partitioning, that we used as an analogue to test the capabilities for zonation and diffusion determination; and 4) a polished section of the Semarkona ordinary chondrite containing chondules comprised of highly zoned and rimmed olivines and pyroxenes in a complex mesostasis of sub-micrometer pyroxenes and glass. The results of these analyses that we will present confirmed our optimism regarding the new analytical capabilities of a field emission microprobe. We were able, at reduced voltages, to accurately analyze the major and minor element composition of intergrowth and rimming phases as small as 200 nm without artifact contribution from the surrounding phases. We were able to determine the compositional gradients at kamacite-taenite boundaries in the pallasite specimen with a resolution of ~180 nm, enabling much higher precision and accuracy determination of the meteorite's cooling rate than previously possible with microprobe measurements. We were able to determine the composition and zonation of phases in the experimental run product, none of which were large enough to be analyzable in a conventional electron microprobe.

An SU-8-based microprobe with a nanostructured surface enhances neuronal cell attachment and growth

NASA Astrophysics Data System (ADS)

Kim, Eunhee; Kim, Jin-Young; Choi, Hongsoo

2017-12-01

Microprobes are used to repair neuronal injury by recording electrical signals from neuronal cells around the surface of the device. Following implantation into the brain, the immune response results in formation of scar tissue around the microprobe. However, neurons must be in close proximity to the microprobe to enable signal recording. A common reason for failure of microprobes is impaired signal recording due to scar tissue, which is not related to the microprobe itself. Therefore, the device-cell interface must be improved to increase the number of neurons in contact with the surface. In this study, we developed nanostructured SU-8 microprobes to support neuronal growth. Nanostructures of 200 nm diameter and depth were applied to the surface of microprobes, and the attachment and neurite outgrowth of PC12 cells on the microprobes were evaluated. Neuronal attachment and neurite outgrowth on the nanostructured microprobes were significantly greater than those on non-nanostructured microprobes. The enhanced neuronal attachment and neurite outgrowth on the nanostructured microprobes occurred in the absence of an adhesive coating, such as poly- l-lysine, and so may be useful for implantable devices for long-term use. Therefore, nanostructured microprobes can be implanted without adhesive coating, which can cause problems in vivo over the long term.

Quantitative simultaneous multi-element microprobe analysis using combined wavelength and energy dispersive systems

NASA Technical Reports Server (NTRS)

Walter, L. S.; Doan, A. S., Jr.; Wood, F. M., Jr.; Bredekamp, J. H.

1972-01-01

A combined WDS-EDS system obviates the severe X-ray peak overlap problems encountered with Na, Mg, Al and Si common to pure EDS systems. By application of easily measured empirical correction factors for pulse pile-up and peak overlaps which are normally observed in the analysis of silicate minerals, the accuracy of analysis is comparable with that expected for WDS electron microprobe analyses. The continuum backgrounds are subtracted for the spectra by a spline fitting technique based on integrated intensities between the peaks. The preprocessed data are then reduced to chemical analyses by existing data reduction programs.

Quantitative measurement of indomethacin crystallinity in indomethacin-silica gel binary system using differential scanning calorimetry and X-ray powder diffractometry.

PubMed

Pan, Xiaohong; Julian, Thomas; Augsburger, Larry

2006-02-10

Differential scanning calorimetry (DSC) and X-ray powder diffractometry (XRPD) methods were developed for the quantitative analysis of the crystallinity of indomethacin (IMC) in IMC and silica gel (SG) binary system. The DSC calibration curve exhibited better linearity than that of XRPD. No phase transformation occurred in the IMC-SG mixtures during DSC measurement. The major sources of error in DSC measurements were inhomogeneous mixing and sampling. Analyzing the amount of IMC in the mixtures using high-performance liquid chromatography (HPLC) could reduce the sampling error. DSC demonstrated greater sensitivity and had less variation in measurement than XRPD in quantifying crystalline IMC in the IMC-SG binary system.

Measurement of particle size distribution of soil and selected aggregate sizes using the hydrometer method and laser diffractometry

NASA Astrophysics Data System (ADS)

Guzmán, G.; Gómez, J. A.; Giráldez, J. V.

2010-05-01

Soil particle size distribution has been traditionally determined by the hydrometer or the sieve-pipette methods, both of them time consuming and requiring a relatively large soil sample. This might be a limitation in situations, such as for instance analysis of suspended sediment, when the sample is small. A possible alternative to these methods are the optical techniques such as laser diffractometry. However the literature indicates that the use of this technique as an alternative to traditional methods is still limited, because the difficulty in replicating the results obtained with the standard methods. In this study we present the percentages of soil grain size determined using laser diffractometry within ranges set between 0.04 - 2000 μm. A Beckman-Coulter ® LS-230 with a 750 nm laser beam and software version 3.2 in five soils, representative of southern Spain: Alameda, Benacazón, Conchuela, Lanjarón and Pedrera. In three of the studied soils (Alameda, Benacazón and Conchuela) the particle size distribution of each aggregate size class was also determined. Aggregate size classes were obtained by dry sieve analysis using a Retsch AS 200 basic ®. Two hundred grams of air dried soil were sieved during 150 s, at amplitude 2 mm, getting nine different sizes between 2000 μm and 10 μm. Analyses were performed by triplicate. The soil sample preparation was also adapted to our conditions. A small amount each soil sample (less than 1 g) was transferred to the fluid module full of running water and disaggregated by ultrasonication at energy level 4 and 80 ml of sodium hexametaphosphate solution during 580 seconds. Two replicates of each sample were performed. Each measurement was made for a 90 second reading at a pump speed of 62. After the laser diffractometry analysis, each soil and its aggregate classes were processed calibrating its own optical model fitting the optical parameters that mainly depends on the color and the shape of the analyzed particle. As a second alternative a unique optical model valid for a broad range of soils developed by the Department of Soil, Water, and Environmental Science of the University of Arizona (personal communication, already submitted) was tested. The results were compared with the particle size distribution measured in the same soils and aggregate classes using the hydrometer method. Preliminary results indicate a better calibration of the technique using the optical model of the Department of Soil, Water, and Environmental Science of the University of Arizona, which obtained a good correlations (r2>0.85). This result suggests that with an appropriate calibration of the optical model laser diffractometry might provide a reliable soil particle characterization.

Ion microprobe measurement of strontium isotopes in calcium carbonate with application to salmon otoliths

USGS Publications Warehouse

Weber, P.K.; Bacon, C.R.; Hutcheon, I.D.; Ingram, B.L.; Wooden, J.L.

2005-01-01

The ion microprobe has the capability to generate high resolution, high precision isotopic measurements, but analysis of the isotopic composition of strontium, as measured by the 87Sr/ 86Sr ratio, has been hindered by isobaric interferences. Here we report the first high precision measurements of 87Sr/ 86Sr by ion microprobe in calcium carbonate samples with moderate Sr concentrations. We use the high mass resolving power (7000 to 9000 M.R.P.) of the SHRIMP-RG ion microprobe in combination with its high transmission to reduce the number of interfering species while maintaining sufficiently high count rates for precise isotopic measurements. The isobaric interferences are characterized by peak modeling and repeated analyses of standards. We demonstrate that by sample-standard bracketing, 87Sr/86Sr ratios can be measured in inorganic and biogenic carbonates with Sr concentrations between 400 and 1500 ppm with ???2??? external precision (2??) for a single analysis, and subpermil external precision with repeated analyses. Explicit correction for isobaric interferences (peak-stripping) is found to be less accurate and precise than sample-standard bracketing. Spatial resolution is ???25 ??m laterally and 2 ??m deep for a single analysis, consuming on the order of 2 ng of material. The method is tested on otoliths from salmon to demonstrate its accuracy and utility. In these growth-banded aragonitic structures, one-week temporal resolution can be achieved. The analytical method should be applicable to other calcium carbonate samples with similar Sr concentrations. Copyright ?? 2005 Elsevier Ltd.

Bioimaging of cells and tissues using accelerator-based sources.

PubMed

Petibois, Cyril; Cestelli Guidi, Mariangela

2008-07-01

A variety of techniques exist that provide chemical information in the form of a spatially resolved image: electron microprobe analysis, nuclear microprobe analysis, synchrotron radiation microprobe analysis, secondary ion mass spectrometry, and confocal fluorescence microscopy. Linear (LINAC) and circular (synchrotrons) particle accelerators have been constructed worldwide to provide to the scientific community unprecedented analytical performances. Now, these facilities match at least one of the three analytical features required for the biological field: (1) a sufficient spatial resolution for single cell (< 1 mum) or tissue (<1 mm) analyses, (2) a temporal resolution to follow molecular dynamics, and (3) a sensitivity in the micromolar to nanomolar range, thus allowing true investigations on biological dynamics. Third-generation synchrotrons now offer the opportunity of bioanalytical measurements at nanometer resolutions with incredible sensitivity. Linear accelerators are more specialized in their physical features but may exceed synchrotron performances. All these techniques have become irreplaceable tools for developing knowledge in biology. This review highlights the pros and cons of the most popular techniques that have been implemented on accelerator-based sources to address analytical issues on biological specimens.

Experimental determination of growth rate effect on U 6+ and Mg 2+ partitioning between aragonite and fluid at elevated U 6+ concentration

NASA Astrophysics Data System (ADS)

Gabitov, R. I.; Gaetani, G. A.; Watson, E. B.; Cohen, A. L.; Ehrlich, H. L.

2008-08-01

Results are reported from an experimental study in which the partitioning of U and Mg between aragonite and an aqueous solution were determined as a function of crystal growth rate. Crystals, identified as aragonite by X-ray diffractometry and micro-Raman spectroscopy, were grown by diffusion of CO 2 from an ammonium carbonate source into a calcium-bearing solution at temperatures of 22 and 53 °C. Hemispherical bundles (spherulites) of aragonite crystals were produced, the growth rates of which decreased monotonically from the spherulite interiors to the edges and thus provide the opportunity to examine the influence of growth rate on crystal composition. Element concentration ratios were measured using electron microprobe (EMP) and fluid composition was determined by inductively coupled plasma-mass spectrometry (ICP-MS) and atomic absorption (AA). Growth rates were determined directly by addition of a Dy spike to the fluid during the experiment that was subsequently located in an experimentally precipitated spherulite using secondary ion mass spectrometry (SIMS). At 22 °C both U/Ca and Mg/Ca partition coefficients exhibited a strong growth rate dependence when crystal growth rates were low, and became independent of growth rate when crystal growth rates were high. The U/Ca ratios in aragonite increase between 22 and 53 °C; in contrast Mg/Ca ratios show inverse dependence on temperature.

A UNIX-based real-time data acquisition system for microprobe analysis using an advanced X11 window toolkit

NASA Astrophysics Data System (ADS)

Kramer, J. L. A. M.; Ullings, A. H.; Vis, R. D.

1993-05-01

A real-time data acquisition system for microprobe analysis has been developed at the Free University of Amsterdam. The system is composed of two parts: a front-end real-time and a back-end monitoring system. The front-end consists of a VMEbus based system which reads out a CAMAC crate. The back-end is implemented on a Sun work station running the UNIX operating system. This separation allows the integration of a minimal, and consequently very fast, real-time executive within the sophisticated possibilities of advanced UNIX work stations.

Age mapping and dating of monazite on the electron microprobe: Deconvoluting multistage tectonic histories

NASA Astrophysics Data System (ADS)

Williams, Michael L.; Jercinovic, Michael J.; Terry, Michael P.

1999-11-01

High-resolution X-ray mapping and dating of monazite on the electron microprobe are powerful geochronological tools for structural, metamorphic, and tectonic analysis. X-ray maps commonly show complex Th, U, and Pb zoning that reflects monazite growth and overgrowth events. Age maps constructed from the X-ray maps simplify the zoning and highlight age domains. Microprobe dating offers a rapid, in situ method for estimating ages of mapped domains. Application of these techniques has placed new constraints on the tectonic history of three areas. In western Canada, age mapping has revealed multiphase monazite, with older cores and younger rims, included in syntectonic garnet. Microprobe ages show that tectonism occurred ca. 1.9 Ga, 700 m.y. later than mylonitization in the adjacent Snowbird tectonic zone. In New Mexico, age mapping and dating show that the dominant fabric and triple-point metamorphism occurred during a 1.4 Ga reactivation, not during the 1.7 Ga Yavapai-Mazatzal orogeny. In Norway, monazite inclusions in garnet constrain high-pressure metamorphism to ca. 405 Ma, and older cores indicate a previously unrecognized component of ca. 1.0 Ga monazite. In all three areas, microprobe dating and age mapping have provided a critical textural context for geochronologic data and a better understanding of the complex age spectra of these multistage orogenic belts.

Advances in Laser Microprobe (U-Th)/He Geochronology

NASA Astrophysics Data System (ADS)

van Soest, M. C.; Monteleone, B. D.; Boyce, J. W.; Hodges, K. V.

2008-12-01

The development of the laser microprobe (U-Th)/He dating method has the potential to overcome many of the limitations that affect conventional (U-Th)/He geochronology. Conventional single- or multi-crystal (U- Th)/He geochronology requires the use of pristine, inclusion-free, euhedral crystals. Furthermore, the ages that are obtained require corrections for the effects of zoning and alpha ejection based on an ensemble of assumptions before interpretation of their geological relevance is possible. With the utilization of microbeam techniques many of the limitations of conventional (U-Th)/He geochronology can either be eliminated by careful spot selection or accounted for by detailed depth profiling analyses of He, U and Th on the same crystal. Combined He, Th, and U depth profiling on the same crystal potentially even offers the ability to extract thermal histories from the analyzed grains. Boyce et al. (2006) first demonstrated the laser microprobe (U-Th)/He dating technique by successfully dating monazite crystals using UV laser ablation to liberate He and determined U and Th concentrations using a Cameca SX-Ultrachron microprobe. At Arizona State University, further development of the microprobe (U-Th)/He dating technique continues using an ArF Excimer laser connected to a GVI Helix Split Flight Tube noble gas mass spectrometer for He analysis and SIMS techniques for U and Th. The Durango apatite age standard has been successfully dated at 30.7 +/- 1.7 Ma (2SD). Work on dating zircons by laser ablation is currently underway, with initial results from Sri Lanka zircon at 437 +/- 14 Ma (2SD) confirmed by conventional (U-Th)/He analysis and in agreement with the published (U-Th)/He age of 443 +/- 9 Ma (2SD) for zircons from this region in Sri Lanka (Nasdala et al., 2004). The results presented here demonstrate the laser microprobe (U-Th)/He method as a powerful tool that allows application of (U- Th)/He dating to areas of research such as detrital apatite and zircon dating, where conventional (U-Th)/He geochronology has limited applicability. Boyce et al. (2006) GCA 70 (3031-3039), Nasdala et al. (2004) Am. Min. 89 (219-231)

Correlated petrographic, electron microprobe, and ion microprobe studies of selected primitive and processed phase assemblages in meteorites

NASA Technical Reports Server (NTRS)

Albee, Arden L.

1993-01-01

During the past three years we have received support to continue our research in elucidating the formation and alteration histories of selected meteoritic materials by a combination of petrographic, trace element, and isotopic analyses employing optical and scanning electron microscopes and electron and ion microprobes. The awarded research funds enabled the P.I. to attend the annual LPSC, the co-I to devote approximately 15 percent of his time to the research proposed in the grant, and partial support for a visiting summer post-doctoral fellow to conduct electron microprobe analyses of meteoritic samples in our laboratory. The research funds, along with support from the NASA Education Initiative awarded to P.I. G. Wasserburg, enabled the co-I to continue a mentoring program with inner-city minority youth. The support enabled us to achieve significant results in the five projects that we proposed (in addition to the Education Initiative), namely: studies of the accretional and post-accretional alteration and thermal histories in CV meteorites, characterization of periclase-bearing Fremdlinge in CV meteorites, characterization of Ni-Pt-Ge-Te-rich Fremdlinge in CV meteorites in an attempt to determine the constraints they place on the petrogenetic and thermal histories of their host CAI's, correlated electron and ion microprobe studies of silicate and phosphate inclusions in the Colomera meteorite in an attempt to determine the petrogenesis of the IE iron meteorites, and development of improved instrumental and correction procedures for improved accuracy of analysis of meteoritic materials with the electron microprobe. This grant supported, in part or whole, 18 publications so far by our research team, with at least three more papers anticipated. The list of these publications is included. The details of the research results are briefly summarized.

Analysis of synthetic diamond single crystals by X-ray topography and double-crystal diffractometry

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

Prokhorov, I. A., E-mail: igor.prokhorov@mail.ru; Ralchenko, V. G.; Bolshakov, A. P.

2013-12-15

Structural features of diamond single crystals synthesized under high pressure and homoepitaxial films grown by chemical vapor deposition (CVD) have been analyzed by double-crystal X-ray diffractometry and topography. The conditions of a diffraction analysis of diamond crystals using Ge monochromators have been optimized. The main structural defects (dislocations, stacking faults, growth striations, second-phase inclusions, etc.) formed during crystal growth have been revealed. The nitrogen concentration in high-pressure/high-temperature (HPHT) diamond substrates is estimated based on X-ray diffraction data. The formation of dislocation bundles at the film-substrate interface in the epitaxial structures has been revealed by plane-wave topography; these dislocations are likelymore » due to the relaxation of elastic macroscopic stresses caused by the lattice mismatch between the substrate and film. The critical thicknesses of plastic relaxation onset in CVD diamond films are calculated. The experimental techniques for studying the real diamond structure in optimizing crystal-growth technology are proven to be highly efficient.« less

Ion microprobe mass analysis of lunar samples. Lunar sample program

NASA Technical Reports Server (NTRS)

Anderson, C. A.; Hinthorne, J. R.

1971-01-01

Mass analyses of selected minerals, glasses and soil particles of lunar, meteoritic and terrestrial rocks have been made with the ion microprobe mass analyzer. Major, minor and trace element concentrations have been determined in situ in major and accessory mineral phases in polished rock thin sections. The Pb isotope ratios have been measured in U and Th bearing accessory minerals to yield radiometric age dates and heavy volatile elements have been sought on the surfaces of free particles from Apollo soil samples.

Electron Microprobe Analyses of Lithic Fragments and Their Minerals from Luna 20 Fines

NASA Technical Reports Server (NTRS)

Conrad, G. H.; Hlava, P. F.; Green, J. A.; Moore, R. B.; Moreland, G.; Dowty, E.; Prinz, M.; Keil, K.; Nehru, C. E.; Bunch, T. E.

1973-01-01

The bulk analyses (determined with the broad beam electron microprobe technique) of lithic fragments are given in weight percentages and are arranged according to the rock classification. Within each rock group the analyses are arranged in order of increasing FeO content. Thin section and lithic fragment numbers are given at the top of each column of analysis and correspond to the numbers recorded on photo mosaics on file in the Institute of Meteoritics. CIPW molecular norms are given for each analysis. Electron microprobe mineral analyses (given in oxide weight percentages), structural formulae and molecular end member values are presented for plagioclase, olivine, pyroxene and K-feldspar. The minerals are selected mostly from lithic fragments that were also analyzed for bulk composition. Within each mineral group the analyses are presented according to the section number and lithic fragment number. Within each lithic fragment the mineral analyses are arranged as follows: Plagioclase in order of increasing CaO; olivine and pyroexene in order of increasing FeO; and K-feldspar in order of increasing K2O. The mineral grains are identified at the top of each column of analysis by grain number and lithic fragment number.

Stanford-USGS shrimp-RG ion microprobe: A new approach to determining the distribution of trace elements in coal

USGS Publications Warehouse

Kolker, A.; Wooden, J.L.; Persing, H.M.; Zielinski, R.A.

2000-01-01

The distribution of Cr and other trace metals of environmental interest in a range of widely used U.S. coals was investigated using the Stanford-USGS SHRIMP-RG ion microprobe . Using the oxygen ion source, concentrations of Cr (11 to 176 ppm), V (23 to 248 ppm), Mn (2 to 149 ppm), Ni (2 to 30 ppm), and 13 other elements were determined in illite/smectite, a group of clay minerals commonly present in coal. The results confirm previous indirect or semi-quantitative determinations indicating illite/smectite to be an important host of these metals. Calibration was achieved using doped aluminosilicate-glass synthetic standards and glasses prepared from USGS rock standards. Grains for analysis were identified optically, and confirmed by 1) precursory electron microprobe analysis and wavelength-dispersive compositional mapping, and 2) SHRIMP-RG major element data obtained concurrently with trace element results. Follow-up investigations will focus on the distribution of As and other elements that are more effectively ionized with the cesium primary beam currently being tested.

The Review of Nuclear Microscopy Techniques: An Approach for Nondestructive Trace Elemental Analysis and Mapping of Biological Materials.

PubMed

Mulware, Stephen Juma

2015-01-01

The properties of many biological materials often depend on the spatial distribution and concentration of the trace elements present in a matrix. Scientists have over the years tried various techniques including classical physical and chemical analyzing techniques each with relative level of accuracy. However, with the development of spatially sensitive submicron beams, the nuclear microprobe techniques using focused proton beams for the elemental analysis of biological materials have yielded significant success. In this paper, the basic principles of the commonly used microprobe techniques of STIM, RBS, and PIXE for trace elemental analysis are discussed. The details for sample preparation, the detection, and data collection and analysis are discussed. Finally, an application of the techniques to analysis of corn roots for elemental distribution and concentration is presented.

Trace elemental analysis of bituminuos coals using the Heidelberg proton microprobe

USGS Publications Warehouse

Chen, J.R.; Kneis, H.; Martin, B.; Nobiling, R.; Traxel, K.; Chao, E.C.T.; Minkin, J.A.

1981-01-01

Trace elements in coal can occur as components of either the organic constituents (macerals) or the inorganic constituents (minerals). Studies of the concentrations and distribution of the trace elements are vital to understanding the geochemical millieu in which the coal was formed and in evaluating the attempts to recover rare but technologically valuable metals. In addition, information on the trace element concentrations is important in predicting the environmental impact of burning particular coals, as many countries move toward greater utilization of coal reserves for energy production. Traditionally, the optical and the electron microscopes and more recently the electron microprobe have been used in studying the components of coal. The proton-induced X-ray emission (PIXE) microprobe offers a new complementary approach with an order of magnitude or more better minimum detection limit. We present the first measurements with a PIXE microprobe of the trace element concentrations of bituminous coal samples. Elemental analyses of the coal macerals-vitrinite, exinite, and inertinite-are discussed for three coal samples from the Eastern U.S.A., three samples from the Western U.S.A., and one sample from the Peoples Republic of China. ?? 1981.

Calibration Issues and Operating System Requirements for Electron-Probe Microanalysis

NASA Technical Reports Server (NTRS)

Carpenter, P.

2006-01-01

Instrument purchase requirements and dialogue with manufacturers have established hardware parameters for alignment, stability, and reproducibility, which have helped improve the precision and accuracy of electron microprobe analysis (EPMA). The development of correction algorithms and the accurate solution to quantitative analysis problems requires the minimization of systematic errors and relies on internally consistent data sets. Improved hardware and computer systems have resulted in better automation of vacuum systems, stage and wavelength-dispersive spectrometer (WDS) mechanisms, and x-ray detector systems which have improved instrument stability and precision. Improved software now allows extended automated runs involving diverse setups and better integrates digital imaging and quantitative analysis. However, instrumental performance is not regularly maintained, as WDS are aligned and calibrated during installation but few laboratories appear to check and maintain this calibration. In particular, detector deadtime (DT) data is typically assumed rather than measured, due primarily to the difficulty and inconvenience of the measurement process. This is a source of fundamental systematic error in many microprobe laboratories and is unknown to the analyst, as the magnitude of DT correction is not listed in output by microprobe operating systems. The analyst must remain vigilant to deviations in instrumental alignment and calibration, and microprobe system software must conveniently verify the necessary parameters. Microanalysis of mission critical materials requires an ongoing demonstration of instrumental calibration. Possible approaches to improvements in instrument calibration, quality control, and accuracy will be discussed. Development of a set of core requirements based on discussions with users, researchers, and manufacturers can yield documents that improve and unify the methods by which instruments can be calibrated. These results can be used to continue improvements of EPMA.

Microprobe studies of microtomed particles of white druse salts in shergottite EETA 79001

NASA Technical Reports Server (NTRS)

Lindstrom, D. J.

1991-01-01

The white druse material in Antarctic shergottite EETA 79001 has attracted much attention as a possible sample fo Martian aqueous deposits. Instrumental Neutron Activation Analysis (INAA) was used to determine trace element analyses of small particles of this material obtained by handpicking of likely grains from broken surfaces of the meteorite. Electron microprobe work was attempted on grain areas as large as 150x120 microns. Backscattered electron images show considerable variations in brightness, and botryoidal structures were observed. Microprobe analyses showed considerable variability both within single particles and between different particles. Microtomed surfaces of small selected particles were shown to be very useful in obtaining information on the texture and composition of rare lithologies like the white druse of EETA 79001. This material is clearly heterogeneous on all distance scales, so a large number of further analyses will be required to characterize it.

Ion microprobe analysis of {sup 18}O/{sup 16}O in authigenic and detrital quartz in the St. Peter Sandstone, Michigan Basin and Wisconsin Arch, USA: Contrasting diagenetic histories

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

Graham, C.M.; Valley, J.W.; Winter, B.L.

1996-12-01

The oxygen isotopic compositions of authigenic quartz cements in sandstones provide a monitor of the temperatures, compositions, and origins of pore-occluding fluids during diagenesis, but quartz overgrowths are too fine-grained to be amenable to conventional isotopic analysis. We have used a Cameca ims-4f ion microprobe to determine oxygen isotopic variations in authigenic and detrital quartz in four samples of the Ordovician St. Peter Sandstone from the Michigan Basin and Wisconsin Arch, midwestern USA. Ion microprobe isotopic analyses have been successfully accomplished with an internal precision of {+-}1{per_thousand} (1{sigma}) and a spatial resolution of 20-30 {mu}m at low mass resolution usingmore » a high voltage offset technique. Repeated analyses of the quartz standard demonstrate a reproducibility of close to {+-}1{per_thousand} (1 sd) in good agreement with that expected from counting statistics. Conventional and ion microprobe analyses are mutually consistent, supporting the accuracy of the ion microprobe analyses. Within-sample isotopic variations of up to 13{per_thousand} and micro-scale isotopic variations of at least 4{per_thousand} over a distance of 100 {mu}m have been measured within quartz overgrowths in a sandstone from the Wisconsin Arch. Overgrowths are uniformly higher in {delta}{sup 18}O than detrital grains, and gradients of up to 25% exist across a few microns. {sup 18}O-enriched quartz overgrowths in sandstones from the Wisconsin Arch show complex CL zonation and reflect one of two possible processes: (1) low-temperature quartz precipitation during mixing of meteoric waters with upwelling basinal fluids; (2) higher temperature quartz precipitation during episodic gravity-driven upwelling of warm basinal fluids (of comparable isotopic composition to Michigan Basin fluids) from the Illinois Basin, related to evolution of Mississippi Valley type Pb-Zn ore-forming fluids. 59 refs., 7 figs., 4 tabs.« less

Cometary and interstellar dust grains - Analysis by ion microprobe mass spectrometry and other techniques

NASA Technical Reports Server (NTRS)

Zinner, Ernst

1991-01-01

A survey of microanalytical measurements on interplanetary dust particles (IDPs) and interstellar dust grains from primitive meteorites is presented. Ion-microprobe mass spectrometry with its capability to determine isotopic compositions of many elements on a micron spatial scale has played a special role. Examples are measurements of H, N, and O isotopes and refractory trace elements in IDPs; C, N, Mg, and Si isotopes in interstellar SiC grains; and C and N isotopes and H, N, Al, and Si concentrations in interstellar graphite grains.

The new confocal heavy ion microprobe beamline at ANSTO: The first microprobe resolution tests and applications for elemental imaging and analysis

NASA Astrophysics Data System (ADS)

Pastuovic, Z.; Siegele, R.; Cohen, D. D.; Mann, M.; Ionescu, M.; Button, D.; Long, S.

2017-08-01

The Centre for Accelerator Science facility at ANSTO has been expanded with the new NEC 6 MV ;SIRIUS; accelerator system in 2015. In this paper we present a detailed description of the new nuclear microprobe-Confocal Heavy Ion Micro-Probe (CHIMP) together with results of the microprobe resolution testing and the elemental analysis performed on typical samples of mineral ore deposits and hyper-accumulating plants regularly measured at ANSTO. The CHIMP focusing and scanning systems are based on the OM-150 Oxford quadrupole triplet and the OM-26 separated scan-coil doublet configurations. A maximum ion rigidity of 38.9 amu-MeV was determined for the following nuclear microprobe configuration: the distance from object aperture to collimating slits of 5890 mm, the working distance of 165 mm and the lens bore diameter of 11 mm. The overall distance from the object to the image plane is 7138 mm. The CHIMP beamline has been tested with the 3 MeV H+ and 6 MeV He2+ ion beams. The settings of the object and collimating apertures have been optimized using the WinTRAX simulation code for calculation of the optimum acceptance settings in order to obtain the highest possible ion current for beam spot sizes of 1 μm and 5 μm. For optimized aperture settings of the CHIMP the beam brightness was measured to be ∼0.9 pA μm-2 mrad-2 for 3 MeV H+ ions, while the brightness of ∼0.4 pA μm-2 mrad-2 was measured for 6 MeV He2+ ions. The smallest beam sizes were achieved using a microbeam with reduced particle rate of 1000 Hz passing through the object slit apertures several micrometers wide. Under these conditions a spatial resolution of ∼0.6 μm × 1.5 μm for 3 MeV H+ and ∼1.8 μm × 1.8 μm for 6 MeV He2+ microbeams in horizontal (and vertical) dimension has been achieved. The beam sizes were verified using STIM imaging on 2000 and 1000 mesh Cu electron microscope grids.

Super-achromatic microprobe for ultrahigh-resolution endoscopic OCT imaging at 800 nm (Conference Presentation)

NASA Astrophysics Data System (ADS)

Yuan, Wu; Alemohammad, Milad; Yu, Xiaoyun; Yu, Shaoyong; Li, Xingde

2016-03-01

In this paper, we report a super-achromatic microprobe made with fiber-optic ball lens to enable ultrahigh-resolution endoscopic OCT imaging. An axial resolution of ~2.4 µm (in air) can be achieved with a 7-fs Ti:Sapphire laser. The microprobe has minimal astigmatism which affords a high transverse resolution of ~5.6 µm. The miniaturized microprobe has an outer diameter of ~520 µm including the encasing metal guard and can be used to image small luminal organs. The performance of the ultrahigh-resolution OCT microprobe was demonstrated by imaging rat esophagus, guinea pig esophagus, and mouse rectum in vivo.

Precession technique and electron diffractometry as new tools for crystal structure analysis and chemical bonding determination.

PubMed

Avilov, A; Kuligin, K; Nicolopoulos, S; Nickolskiy, M; Boulahya, K; Portillo, J; Lepeshov, G; Sobolev, B; Collette, J P; Martin, N; Robins, A C; Fischione, P

2007-01-01

We have developed a new fast electron diffractometer working with high dynamic range and linearity for crystal structure determinations. Electron diffraction (ED) patterns can be scanned serially in front of a Faraday cage detector; the total measurement time for several hundred ED reflections can be tens of seconds having high statistical accuracy for all measured intensities (1-2%). This new tool can be installed to any type of TEM without any column modification and is linked to a specially developed electron beam precession "Spinning Star" system. Precession of the electron beam (Vincent-Midgley technique) reduces dynamical effects allowing also use of accurate intensities for crystal structure analysis. We describe the technical characteristics of this new tool together with the first experimental results. Accurate measurement of electron diffraction intensities by electron diffractometer opens new possibilities not only for revealing unknown structures, but also for electrostatic potential determination and chemical bonding investigation. As an example, we present detailed atomic bonding information of CaF(2) as revealed for the first time by precise electron diffractometry.

Soil Particle Size Analysis by Laser Diffractometry: Result Comparison with Pipette Method

NASA Astrophysics Data System (ADS)

Šinkovičová, Miroslava; Igaz, Dušan; Kondrlová, Elena; Jarošová, Miriam

2017-10-01

Soil texture as the basic soil physical property provides a basic information on the soil grain size distribution as well as grain size fraction representation. Currently, there are several methods of particle dimension measurement available that are based on different physical principles. Pipette method based on the different sedimentation velocity of particles with different diameter is considered to be one of the standard methods of individual grain size fraction distribution determination. Following the technical advancement, optical methods such as laser diffraction can be also used nowadays for grain size distribution determination in the soil. According to the literature review of domestic as well as international sources related to this topic, it is obvious that the results obtained by laser diffractometry do not correspond with the results obtained by pipette method. The main aim of this paper was to analyse 132 samples of medium fine soil, taken from the Nitra River catchment in Slovakia, from depths of 15-20 cm and 40-45 cm, respectively, using laser analysers: ANALYSETTE 22 MicroTec plus (Fritsch GmbH) and Mastersizer 2000 (Malvern Instruments Ltd). The results obtained by laser diffractometry were compared with pipette method and the regression relationships using linear, exponential, power and polynomial trend were derived. Regressions with the three highest regression coefficients (R2) were further investigated. The fit with the highest tightness was observed for the polynomial regression. In view of the results obtained, we recommend using the estimate of the representation of the clay fraction (<0.01 mm) polynomial regression, to achieve a highest confidence value R2 at the depths of 15-20 cm 0.72 (Analysette 22 MicroTec plus) and 0.95 (Mastersizer 2000), from a depth of 40-45 cm 0.90 (Analysette 22 MicroTec plus) and 0.96 (Mastersizer 2000). Since the percentage representation of clayey particles (2nd fraction according to the methodology of Complex Soil Survey done in Slovakia) in soil is the determinant for soil type specification, we recommend using the derived relationships in soil science when the soil texture analysis is done according to laser diffractometry. The advantages of laser diffraction method comprise the short analysis time, usage of small sample amount, application for the various grain size fraction and soil type classification systems, and a wide range of determined fractions. Therefore, it is necessary to focus on this issue further to address the needs of soil science research and attempt to replace the standard pipette method with more progressive laser diffraction method.

Measurement of carbon distribution in nuclear fuel pin cladding specimens by means of a secondary ion mass spectrometer

NASA Astrophysics Data System (ADS)

Bart, Gerhard; Aerne, Ernst Tino; Burri, Martin; Zwicky, Hans-Urs

1986-11-01

Cladding carburization during irradiation of advanced mixed uranium plutonium carbide fast breeder reactor fuel is possibly a life limiting fuel pin factor. The quantitative assessment of such clad carbon embrittlement is difficult to perform by electron microprobe analysis because of sample surface contamination, and due to the very low energy of the carbon K α X-ray transition. The work presented here describes a method developed at the Swiss Federal Institute for Reactor Research (EIR) to use shielded secondary ion mass spectrometry (SIMS) as an accurate tool to determine radial distribution profiles of carbon in radioactive stainless steel fuel pin cladding. Compared with nuclear microprobe analysis (NMA) [1], which is also an accurate method for carbon analysis, the SIMS method distinguishes itself by its versatility for simultaneous determination of additional impurities.

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

Vazehrad, S., E-mail: vazehrad@kth.se; Elfsberg, J., E-mail: jessica.elfsberg@scania.com; Diószegi, A., E-mail: attila.dioszegi@jth.hj.se

An investigation on silicon segregation of lamellar, compacted and nodular graphite iron was carried out by applying a selective, immersion color etching and a modified electron microprobe to study the microstructure. The color etched micrographs of the investigated cast irons by revealing the austenite phase have provided data about the chronology and mechanism of microstructure formation. Moreover, electron microprobe has provided two dimensional segregation maps of silicon. A good agreement was found between the segregation profile of silicon in the color etched microstructure and the silicon maps achieved by electron microprobe analysis. However, quantitative silicon investigation was found to bemore » more accurate than color etching results to study the size of the eutectic colonies. - Highlights: • Sensitivity of a color etchant to silicon segregation is quantitatively demonstrated. • Si segregation measurement by EMPA approved the results achieved by color etching. • Color etched micrographs provided data about solidification mechanism in cast irons. • Austenite grain boundaries were identified by measuring the local Si concentration.« less

A novel technique for producing antibody-coated microprobes using a thiol-terminal silane and a heterobifunctional crosslinker.

PubMed

Routh, V H; Helke, C J

1997-02-01

Antibody-coated microprobes are used to measure neuropeptide release in the central nervous system. Although they are not quantitative, they provide the most precise spatial resolution of the location of in vivo release of any currently available method. Previous methods of coating antibody microprobes are difficult and time-consuming. Moreover, using these methods we were unable to produce evenly coated antibody microprobes. This paper describes a novel method for the production of antibody microprobes using thiol-terminal silanes and the heterobifunctional crosslinker, 4-(4-N-maleimidophenyl)butyric acid hydrazide HCl 1/2 dioxane (MPBH). Following silation, glass micropipettes are incubated with antibody to substance P (SP) that has been conjugated to MPBH. This method results in a dense, even coating of antibody without decreasing the biological activity of the antibody. Additionally, this method takes considerably less time than previously described methods without sacrificing the use of antibody microprobes as micropipettes. The sensitivity of the microprobes for SP is in the picomolar range, and there is a linear correlation between the log of SP concentration (M) and B/B0 (r2 = 0.98). The microprobes are stable for up to 3 weeks when stored in 0.1 M sodium phosphate buffer with 50 mM NaCl (pH 7.4) at 5 degrees C. Finally, insertion into the exposed spinal cord of an anesthetized rat for 15 min produces no damage to the antibody coating.

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

Spatial investigation of some uranium minerals using nuclear microprobe

NASA Astrophysics Data System (ADS)

Valter, Anton A.; Knight, Kim B.; Eremenko, Gelij K.; Magilin, Dmitry V.; Ponomarov, Artem A.; Pisansky, Anatoly I.; Romanenko, Alexander V.; Ponomarev, Alexander G.

2018-01-01

In this work, several individual grains of uranium minerals—uraninite with high content of Ca, Ca-rich boltwoodite, growths of uranophane with β-uranophane, and weeksite—from different uranium deposits were studied by a scanning nuclear microprobe. Particle-induced X-ray emission technique provided by the microprobe (µ-PIXE) was carried out to obtain a concentration and 2D distribution of elements in these minerals. In addition, energy dispersive X-ray spectrometry (SEM-EDS) provided by a scanning electron microscope was used. The types of minerals were determined by X-ray diffraction methods. Results of this study improved the understanding of trace elemental composition of the uranium minerals depending on their origin. Obtained signatures could be linked then to the sample provenance. Such data are important for nuclear forensics to identify the ore types and even specific ore bodies, when only small samples may be available for analysis. In this study, the µ-PIXE technique was used for obtaining the 2D distribution of trace elements that are not commonly measured by SEM-EDS at the relevant concentrations. The detected levels and precisions of elements determination by µ-PIXE were also defined. Using µ-PIXE, several micro mineral inclusions such as phosphate with high level of V and Si were identified. The age of the uranium minerals was estimated due to a significant content of radiogenic Pb that provides an additional parameter for determination of the main attributive characteristics of the minerals. This work also showed that due to its high elemental sensitivity the nuclear microprobe can be a new analytical tool for creating a nuclear forensic database from the known uranium deposits and a subsequent analysis of the intercepted illicit materials.

Spatial investigation of some uranium minerals using nuclear microprobe

NASA Astrophysics Data System (ADS)

Valter, Anton A.; Knight, Kim B.; Eremenko, Gelij K.; Magilin, Dmitry V.; Ponomarov, Artem A.; Pisansky, Anatoly I.; Romanenko, Alexander V.; Ponomarev, Alexander G.

2018-06-01

In this work, several individual grains of uranium minerals—uraninite with high content of Ca, Ca-rich boltwoodite, growths of uranophane with β-uranophane, and weeksite—from different uranium deposits were studied by a scanning nuclear microprobe. Particle-induced X-ray emission technique provided by the microprobe (µ-PIXE) was carried out to obtain a concentration and 2D distribution of elements in these minerals. In addition, energy dispersive X-ray spectrometry (SEM-EDS) provided by a scanning electron microscope was used. The types of minerals were determined by X-ray diffraction methods. Results of this study improved the understanding of trace elemental composition of the uranium minerals depending on their origin. Obtained signatures could be linked then to the sample provenance. Such data are important for nuclear forensics to identify the ore types and even specific ore bodies, when only small samples may be available for analysis. In this study, the µ-PIXE technique was used for obtaining the 2D distribution of trace elements that are not commonly measured by SEM-EDS at the relevant concentrations. The detected levels and precisions of elements determination by µ-PIXE were also defined. Using µ-PIXE, several micro mineral inclusions such as phosphate with high level of V and Si were identified. The age of the uranium minerals was estimated due to a significant content of radiogenic Pb that provides an additional parameter for determination of the main attributive characteristics of the minerals. This work also showed that due to its high elemental sensitivity the nuclear microprobe can be a new analytical tool for creating a nuclear forensic database from the known uranium deposits and a subsequent analysis of the intercepted illicit materials.

Crystal and Vibrational Structure of Energetic 3,5-dinitro 1,3,5-oxadiazinane (DOD) by Single Crystal X-ray Diffractometry and Raman Spectroscopy

DTIC Science & Technology

2018-03-19

calculations using a temperature of 298 K. 15. SUBJECT TERMS 3,5-dinitro-1,3,5-oxadiazinane (DOD), X-ray crystallography , Raman, energetic material...X-ray analysis. 2.2 Characterization X-ray Crystallography . DOD crystals were characterized with a SuperNova, Dualflex, EosS2 diffractometer using

Ion microprobe magnesium isotope analysis of plagioclase and hibonite from ordinary chondrites

NASA Technical Reports Server (NTRS)

Hinton, R. W.; Bischoff, A.

1984-01-01

Ion and electron microprobes were used to examine Mg-26 excesses from Al-26 decay in four Al-rich objects from the type 3 ordinary hibonite clast in the Dhajala chondrite. The initial Al-26/Al-27 ratio was actually significantly lower than Al-rich inclusions in carbonaceous chondrites. Also, no Mg-26 excesses were found in three plagioclase-bearing chondrules that were also examined. The Mg-26 excesses in the hibonite chondrites indicated a common origin for chondrites with the excesses. The implied Al-26 content in a proposed parent body could not, however, be confirmed as a widespread heat source in the early solar system.

In vivo deployment of mechanically adaptive nanocomposites for intracortical microelectrodes

PubMed Central

Harris, J P; Hess, A E; Rowan, S J; Weder, C; Zorman, C A; Tyler, D J; Capadona, J R

2012-01-01

We recently introduced a series of stimuli-responsive, mechanically-adaptive polymer nanocomposites. Here, we report the first application of these bio-inspired materials as substrates for intracortical microelectrodes. Our hypothesis is that the ideal electrode should be initially stiff to facilitate minimal trauma during insertion into the cortex, yet becomes mechanically compliant to match the stiffness of the brain tissue and minimize forces exerted on the tissue, attenuating inflammation. Microprobes created from mechanically reinforced nanocomposites demonstrated a significant advantage compared to model microprobes composed of neat polymer only. The nanocomposite microprobes exhibit a higher storage modulus (E’ = ~5 GPa) than the neat polymer microprobes (E’ = ~2 GPa) and could sustain higher loads (~17 mN), facilitating penetration through the pia mater and insertion into the cerebral cortex of a rat. In contrast, the neat polymer microprobes mechanically failed under lower loads (~7 mN) before they were capable of inserting into cortical tissue. Further, we demonstrated the material’s ability to morph while in the rat cortex to more closely match the mechanical properties of the cortical tissue. Nanocomposite microprobes that were implanted into the rat cortex for up to 8 weeks demonstrated increased cell density at the microelectrode-tissue interface and a lack of tissue necrosis or excessive gliosis. This body of work introduces our nanocomposite-based microprobes as adaptive substrates for intracortical microelectrodes and potentially other biomedical applications. PMID:21654037

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

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

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

The electron microprobe as a metallographic tool

NASA Technical Reports Server (NTRS)

Goldstein, J. I.

1974-01-01

The electron microprobe (EMP) is shown to represent one of the most powerful techniques for the examination of the microstructure of materials. It is an electron optical instrument in which compositional and topographic information is obtained from regions smaller than 1 micron in diameter on a specimen. Photographs of compositional and topographic changes in 1-sq-mm to 20-sq-micron areas on various types of specimens can also be obtained. These photographs are strikingly similar to optical photomicrographs. Various signals measured in the EMP (X-rays, secondary electrons, backscattered electrons, etc.) are discussed, along with their resolution and the type of information they may help obtain. In addition to elemental analysis, solid state detecting and scanning techniques are reviewed. Various techniques extending the EMP instrument capabilities, such as deconvolution and soft X-ray analysis, are also described.

On the Applications of IBA Techniques to Biological Samples Analysis: PIXE and RBS

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

Falcon-Gonzalez, J. M.; Bernal-Alvarado, J.; Sosa, M.

2008-08-11

The analytical techniques based on ion beams or IBA techniques give quantitative information on elemental concentration in samples of a wide variety of nature. In this work, we focus on PIXE technique, analyzing thick target biological specimens (TTPIXE), using 3 MeV protons produced by an electrostatic accelerator. A nuclear microprobe was used performing PIXE and RBS simultaneously, in order to solve the uncertainties produced in the absolute PIXE quantifying. The advantages of using both techniques and a nuclear microprobe are discussed. Quantitative results are shown to illustrate the multielemental resolution of the PIXE technique; for this, a blood standard wasmore » used.« less

SU-8 microprobe with microelectrodes for monitoring electrical impedance in living tissues.

PubMed

Tijero, M; Gabriel, G; Caro, J; Altuna, A; Hernández, R; Villa, R; Berganzo, J; Blanco, F J; Salido, R; Fernández, L J

2009-04-15

This paper presents a minimally invasive needle-shaped probe capable of monitoring the electrical impedance of living tissues. This microprobe consists of a 160 microm thick SU-8 substrate containing four planar platinum (Pt) microelectrodes. We design the probe to minimize damage to the surrounding tissue and to be stiff enough to be inserted in living tissues. The proposed batch fabrication process is low cost and low time consuming. The microelectrodes obtained with this process are strongly adhered to the SU-8 substrate and their impedance does not depend on frequency variation. In vitro experiments are compared with previously developed Si and SiC based microprobes and results suggest that it is preferable to use the SU-8 based microprobes due to their flexibility and low cost. The microprobe is assembled on a flexible printed circuit FPC with a conductive glue, packaged with epoxy and wired to the external instrumentation. This flexible probe is inserted into a rat kidney without fracturing and succeeds in demonstrating the ischemia monitoring.

Microprobe Analysis of Pu-Ga Standards

DOE PAGES

Wall, Angélique D.; Romero, Joseph P.; Schwartz, Daniel

2017-08-04

In order to obtain quantitative analysis using an Electron Scanning Microprobe it is essential to have a standard of known composition. Most elemental and multi-elemental standards can be easily obtained from places like Elemental Scientific or other standards organizations that are NIST (National Institute of Standards and Technology) traceable. It is, however, more challenging to find standards for plutonium. Past work performed in our group has typically involved using the plutonium sample to be analysed as its own standard as long as all other known components of the sample have standards to be compared to [1,2,3]. Finally, this method worksmore » well enough, but this experiment was performed in order to develop a more reliable standard for plutonium using five samples of known chemistry of a plutonium gallium mix that could then be used as the main plutonium and gallium standards for future experiments.« less

Microprobe Analysis of Pu-Ga Standards

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

Wall, Angélique D.; Romero, Joseph P.; Schwartz, Daniel

In order to obtain quantitative analysis using an Electron Scanning Microprobe it is essential to have a standard of known composition. Most elemental and multi-elemental standards can be easily obtained from places like Elemental Scientific or other standards organizations that are NIST (National Institute of Standards and Technology) traceable. It is, however, more challenging to find standards for plutonium. Past work performed in our group has typically involved using the plutonium sample to be analysed as its own standard as long as all other known components of the sample have standards to be compared to [1,2,3]. Finally, this method worksmore » well enough, but this experiment was performed in order to develop a more reliable standard for plutonium using five samples of known chemistry of a plutonium gallium mix that could then be used as the main plutonium and gallium standards for future experiments.« less

Fast probing of glucose and fructose in plant tissues via plasmonic affinity sandwich assay with molecularly-imprinted extraction microprobes.

PubMed

Muhammad, Pir; Liu, Jia; Xing, Rongrong; Wen, Yanrong; Wang, Yijia; Liu, Zhen

2017-12-01

Determination of specific target compounds in agriculture food and natural plant products is essential for many purposes; however, it is often challenging due to the complexity of the sample matrices. Herein we present a new approach called plasmonic affinity sandwich assay for the facile and rapid probing of glucose and fructose in plant tissues. The approach mainly relies on molecularly imprinted plasmonic extraction microprobes, which were prepared on gold-coated acupuncture needles via boronate affinity controllable oriented surface imprinting with the target monosaccharide as the template molecules. An extraction microprobe was inserted into plant tissues under investigation, which allowed for the specific extraction of glucose or fructose from the tissues. The glucose or fructose molecules extracted on the microprobe were labeled with boronic acid-functionalized Raman-active silver nanoparticles, and thus affinity sandwich complexes were formed on the microprobes. After excess Raman nanotags were washed away, the microprobe was subjected to Raman detection. Upon being irradiated with a laser beam, surface plasmon on the gold-coated microprobes was generated, which further produced plasmon-enhanced Raman scattering of the silver-based nanotags and thereby provided sensitive detection. Apple fruits, which contain abundant glucose and fructose, were used as a model of plant tissues. The approach exhibited high specificity, good sensitivity (limit of detection, 1 μg mL -1 ), and fast speed (the whole procedure required only 20 min). The spatial distribution profiles of glucose and fructose within an apple were investigated by the developed approach. Copyright © 2017 Elsevier B.V. All rights reserved.

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.

Characterization and evaluation of miconazole salts and cocrystals for improved physicochemical properties.

PubMed

Tsutsumi, Shunichirou; Iida, Motoo; Tada, Norio; Kojima, Takashi; Ikeda, Yukihiro; Moriwaki, Toshiya; Higashi, Kenjirou; Moribe, Kunikazu; Yamamoto, Keiji

2011-12-15

Miconazole salts and cocrystals were studied to improve the physicochemical properties of miconazole. Maleate, hemifumarate, and hemisuccinate were prepared and characterized by powder X-ray diffractometry, differential scanning calorimetry, and single crystal X-ray diffractometry. The intrinsic dissolution rate and stability of each miconazole crystal form were compared to those of freebase and nitrate to evaluate the optimal crystal form. Crystal structure analysis indicated that maleate was a salt formed by proton transfer from the acid to the imidazole group of miconazole. Hemifumarate and hemisuccinate were determined to be cocrystals formed by hydrogen bonding between the acids and the base in their crystal lattices. Intrinsic dissolution tests showed that the formation of salts and cocrystals improved the dissolution rate of miconazole. Stability tests of preliminary formulations prepared with each crystal form indicated that maleate and hemifumarate were unstable at 80°C and generated a specific degraded product, i.e., a Michael adduct, between miconazole and the acids. Hemisuccinate had a superior intrinsic dissolution rate and stability, and is thus considered a promising crystal form of miconazole. Copyright © 2011 Elsevier B.V. All rights reserved.

Zircon geochronology and ca. 400 Ma exhumation of Norwegian ultrahigh-pressure rocks: An ion microprobe and chemical abrasion study

USGS Publications Warehouse

Root, D.B.; Hacker, B.R.; Mattinson, J.M.; Wooden, J.L.

2004-01-01

Understanding the formation and exhumation of the remarkable ultrahigh-pressure (UHP) rocks of the Western Gneiss Region, Norway, hinges on precise determination of the time of eclogite recrystallization. We conducted detailed thermal ionization mass spectrometry, chemical abrasion analysis and sensitive high-resolution ion-microprobe analysis of zircons from four ultrahigh- and high-pressure (HP) rocks. Ion-microprobe analyses from the Flatraket eclogite yielded a broad range of apparently concordant Caledonian ages, suggesting long-term growth. In contrast, higher precision thermal ionization mass spectrometry analysis of zircon subject to combined thermal annealing and multi-step chemical abrasion yielded moderate Pb loss from the first (lowest temperature) abrasion step, possible minor Pb loss or minor growth at 400 Ma from the second step and a 407-404 Ma cluster of slightly discordant 206Pb/238U ages, most likely free from Pb loss, from the remaining abrasion steps. We interpret the latter to reflect zircon crystallization at ???405-400 Ma with minor discordance from inherited cores. Zircon crystallization occurred at eclogite-facies, possibly post-peak conditions, based on compositions of garnet inclusions in zircon as well as nearly flat HREE profiles and lack of Eu anomalies in zircon fractions subjected to chemical abrasion. These ages are significantly younger than the 425 Ma age often cited for western Norway eclogite recrystallization, implying faster rates of exhumation (>2.5-8.5 km/Myr), and coeval formation of eclogites across the UHP portion of the Western Gneiss Region. ?? 2004 Published by Elsevier B.V.

RN12 and RN30 Epidote anlayses

DOE Data Explorer

Andrew Fowler

2015-01-01

Results for laser ablation measurement of reare earth elments and electron microprobe analysis of major elments in hydrothermal epidote. Laser ablation measurements were completed using an Agilent 7700 quadrupole ICP-MS coupled with 193nm Photon Instruments Excimer laser.

Mineralogical Composition of the Mexican Ordinary Chondrite Type Meteorite: A Raman, Infrared and XRD Study

NASA Astrophysics Data System (ADS)

Ostrooumov, M.

2016-08-01

The Raman microprobe (RMP), infrared (IR) and XRD analysis have been applied to the examination of mineralogical composition of seven mexican meteorites: Aldama, Cosina, El Pozo, Escalon, Nuevo Mercurio,Pacula, Zapotitlan Salinas.

Laser-Raman microprobe identification of inclusions in capsules associated with silicone gel breast implants.

PubMed

Centeno, J A; Mullick, F G; Panos, R G; Miller, F W; Valenzuela-Espinoza, A

1999-07-01

Raman spectroscopy (the analysis of scattered photons after excitation with a monochromatic light source) provides a nondestructive method for identifying organic and inorganic materials on the basis of the molecule's characteristic spectrum of vibrational frequencies. Although the technique has been predominantly applied in sciences other than pathology, the recent advent of high-quality microscope optics coupled to optical Raman spectrometers (a variation known as a Raman microprobe) rendered this technique amenable to applications in human pathology. In the Raman microprobe, a laser beam is focused on a spot approximately 1 microm in diameter on the surface of the sample, e.g., tissue, and the scattered light is collected and analyzed. In this investigation, we used the Raman microprobe for the identification of foreign materials in breast implant capsular tissues. The characteristic silicone group frequencies associated with the silicon-oxygen stretch, the silicone-carbon stretch, the silicon-methyl and the methyl carbon-hydrogen stretch frequencies were used to identify polydimethylsiloxane and to define chemical differences among the various other implant-related inclusions. All of the inclusions were positively identified in a series of 44 capsules from silicone gel-filled implants: polydimethylsiloxane was found in 44 of 44 capsules surrounding silicone gel-filled implants; polyurethane was seen in 4 of 4 capsules around polyurethane foam-coated gel-filled implants; 4 of 4 capsules enveloping Dacron patch gel-filled implants revealed Dacron; and talc was identified in 8 of these 44 capsules. Raman microspectroscopy provides a rapid, accurate, and sensitive method for identifying inclusions associated with silicone and other implant materials in tissue.

Chemical and Isotopic Analysis of Trace Organic Matter on Meteorites and Interstellar Dust Using a Laser Microprobe Instrument

NASA Technical Reports Server (NTRS)

Zare, Richard N.; Boyce, Joseph M. (Technical Monitor)

2001-01-01

Polycyclic Aromatic Hydrocarbons (PAHs) are of considerable interest today because they are ubiquitous on Earth and in the interstellar medium (ISM). In fact, about 20% of cosmic carbon in the galaxy is estimated to be in the form of PAHs. Investigation of these species has obvious uses for determining the cosmochemistry of the solar system. Work in this laboratory has focused on four main areas: 1) Mapping the spatial distribution of PAHs in a variety of meteoritic samples and comparing this distribution with mineralogical features of the meteorite to determine whether a correlation exists between the two. 2) Developing a method for detection of fullerenes in extraterrestrial samples using microprobe Laser Desorption Ionization Mass Spectroscopy and utilizing this technique to investigate fullerene presence, while exploring the possibility of spatially mapping the fullerene distribution in these samples through in situ detection. 3) Investigating a possible formation pathway for meteoritic and ancient terrestrial kerogen involving the photochemical reactions of PAHs with alkanes under prebiotic and astrophysically relevant conditions. 4) Studying reaction pathways and identifying the photoproducts generated during the photochemical evolution of PAH-containing interstellar ice analogs as part of an ongoing collaboration with researchers at the Astrochemistry Lab at NASA Ames. All areas involve elucidation of the solar system formation and chemistry using microprobe Laser Desorption Laser Ionization Mass Spectrometry. A brief description of microprobe Laser Desorption Ionization Mass Spectroscopy, which allows selective investigation of subattomole levels of organic species on the surface of a sample at 10-40 micrometer spatial resolution, is given.

Laboratory technology and cosmochemistry

PubMed Central

Zinner, Ernst K.; Moynier, Frederic; Stroud, Rhonda M.

2011-01-01

Recent developments in analytical instrumentation have led to revolutionary discoveries in cosmochemistry. Instrumental advances have been made along two lines: (i) increase in spatial resolution and sensitivity of detection, allowing for the study of increasingly smaller samples, and (ii) increase in the precision of isotopic analysis that allows more precise dating, the study of isotopic heterogeneity in the Solar System, and other studies. A variety of instrumental techniques are discussed, and important examples of discoveries are listed. Instrumental techniques and instruments include the ion microprobe, laser ablation gas MS, Auger EM, resonance ionization MS, accelerator MS, transmission EM, focused ion-beam microscopy, atom probe tomography, X-ray absorption near-edge structure/electron loss near-edge spectroscopy, Raman microprobe, NMR spectroscopy, and inductively coupled plasma MS. PMID:21498689

Synchrotron X-ray microscopy and spectroscopy analysis of iron in hemochromatosis liver and intestines

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

Ko, J .Y. Peter; Sham, Tsun-Kong; Chakrabarti, Subrata

2009-12-01

Hemochromatosis is a genetic disorder that causes body to store excess iron in organs such as heart or liver. Distribution of iron, as well as copper, zinc and calcium, and chemical identity of iron in hemochromatosis liver and intestine were investigated by X-ray microprobe experiments, which consist of X-ray microscopy and micro-X-ray absorption fine structure. Our results show that iron concentration in hemochromatosis liver tissue is high, while much less Fe is found in intestinal tissue. Moreover, chemical identity of Fe in hemochromatosis liver can be identified. X-ray microprobe experiments allows for examining elemental distribution at an excellent spatial resolution.more » Moreover, chemical identity of element of interest can be obtained.« less

Ion microprobe mass analysis of plagioclase from 'non-mare' lunar samples

NASA Technical Reports Server (NTRS)

Meyer, C., Jr.; Anderson, D. H.; Bradley, J. G.

1974-01-01

The ion microprobe was used to measure the composition and distribution of trace elements in lunar plagioclase, and these analyses are used as criteria in determining the possible origins of some nonmare lunar samples. The Apollo 16 samples with metaclastic texture and high-bulk trace-element contents contain plagioclase clasts with extremely low trace-element contents. These plagioclase inclusions represent unequilibrated relicts of anorthositic, noritic, or troctolitic rocks that have been intermixed as a rock flour into the KREEP-rich matrix of these samples. All of the plagioclase-rich inclusions which were analyzed in the KREEP-rich Apollo 14 breccias were found to be rich in trace elements. This does not seem to be consistent with the interpretation that the Apollo 14 samples represent a pre-Imbrium regolith, because such an ancient regolith should have contained many plagioclase clasts with low trace-element contents more typical of plagioclase from the pre-Imbrium crust. Ion-microprobe analyses for Ba and Sr in large plagioclase phenocrysts in 14310 and 68415 are consistent with the bulk compositions of these rocks and with the known distribution coefficients for these elements. The distribution coefficient for Li (basaltic liquid/plagioclase) was measured to be about 2.

First Evidence of Epithermal Gold Occurrences in the SE Afar Rift, Republic of Djibouti

NASA Astrophysics Data System (ADS)

Moussa, Nima; Fouquet, Yves; Caminiti, Antoine Marie; Le Gall, Bernard; Rolet, Joel; Bohn, Marcel; Etoubleau, Joel; Delacourt, Christophe; Jalludin, Mohamed

2010-05-01

The Republic of Djibouti, located at the SE part of the Afar volcanic Triangle, is characterized by intense tectonic and bimodal volcanic activity, and is emplaced over an earlier magmatic rift system, as old as 25-30 Ma. Each magmatic event is accompanied by hydrothermal activity. Few works have been so far published on hydrothermal mineralization in the Afar area. Mineralization generally occur as veins and are mainly associated with acidic volcanic intrusions along the fractures at the edges of grabens established during the last 4 Ma. Eighty samples from hydrothermal quartz ± carbonate veins and breccias were studied on 9 different sites representative of 4 main volcanic events ranging in age from early Miocene up to Present. Gold was found in excess of 200 ppb in 30% of the samples. Mineralogical analyses based on optical reflected light microscopy, X-Ray diffractometry, X-Ray fluorescence, inductively coupled plasma mass spectroscopy and electron microprobe, led us to identify two types of gold mineralization (i) native gold, electrum, hessite and sulfides (chalcopyrite, pyrite, bornite, ± sphalerite, and galena) in massive quartz breccias and banded chalcedony, (ii) gold, electrum, hematite, magnetite, trace minerals (argentite) and adularia in banded chalcedony. Another group without gold is characterized by quartz, pyrite ± goethite. Secondary minerals are characterized by goethite, native silver and native copper. Arsenic is enriched in pyrite in samples with a high gold content. The bimodal volcanism, the occurrence of adularia, the native gold and electrum in banded silica veins, are classically observed in neutral epithermal systems. The discovery of this type of mineralization in a recent-active continental rift system supplies new insights about hydrothermal processes associated with volcanic activity in a spreading context. Keywords: Republic of Djibouti, Afar Triangle, Hydrothermal, Epithermal system, Gold

FTIR Analysis of Aerogel Keystones from the Stardust Interstellar Dust Collector: Assessment of Terrestrial Organic Contamination and X-Ray Microprobe Beam Damage

NASA Astrophysics Data System (ADS)

Bechtel, H. A.; Allen, C.; Bajt, S.; Borg, J.; Brenker, F.; Bridges, J.; Brownlee, D. E.; Burchell, M.; Burghammer, M.; Butterworth, A. L.; Cloetens, P.; Davis, A. M.; Floss, C.; Flynn, G. J.; Frank, D.; Gainsforth, Z.; Grun, E.; Heck, P. R.; Hillier, J. K.; Hoppe, P.; Howard, L.; Huss, G. R.; Huth, J.; Kearsley, A.; King, A. J.; Lai, B.; Leitner, J.; Lemelle, L.; Leroux, H.; Nittler, L. R.; Ogliore, R. C.; Postberg, F.; Price, M. C.; Sandford, S. A.; Sans Tresseras, J. A.; Schmitz, S.; Schoonjans, T.; Silversmit, G.; Simionovici, A.; Srama, R.; Stadermann, F. J.; Stephan, T.; Stodolna, J.; Stroud, R. M.; Sutton, S. R.; Toucoulou, R.; Trieloff, M.; Tsou, P.; Tsuchiyama, A.; Tyliczszak, T.; Vekemans, B.; Vincze, L.; Westphal, A. J.; Zolensky, M. E.; 29,000 Stardust@Home Dusters

2011-03-01

More than 20 aerogel keystones, many of which contained candidates for interstellar dust, were extracted from the Stardust interstellar dust collector and examined with synchrotron FTIR spectromicroscopy.

The study of voids in the AuAl thin-film system using the nuclear microprobe

NASA Astrophysics Data System (ADS)

de Waal, H. S.; Pretorius, R.; Prozesky, V. M.; Churms, C. L.

1997-07-01

A Nuclear Microprobe (NMP) was used to study void formation in thin film gold-aluminium systems. Microprobe Rutherford Backscattering Spectrometry (μRBS) was utilised to effectively obtain a three-dimensional picture of the void structure on the scale of a few nanometers in the depth dimension and a few microns in the in-plane dimension. This study illustrates the usefulness of the NMP in the study of materials and specifically thin-film structures.

In vivo monitoring of nanosphere onsite delivery using fiber optic microprobe

NASA Astrophysics Data System (ADS)

Lo, Leu-Wei; Yang, Chung-Shi

2005-02-01

To recognize the information of ischemia-induced blood vessel permeability would be valuable to formulate the drugs for optimal local delivery, we constructed an implantable needle type fiber-optic microprobe for the monitoring of in vivo fluorescent substances in anesthetized rats. This fiber-optic microprobe was composed of coaxial optical fibers and catheterized using a thin wall tubing of stainless steel (~400 um O.D. and ~300 um I.D.). The central fiber, with 100 um core diameter and 20 um cladding, coated with a 30 um layer of gold, was surrounded by 10 fibers with 50 um cores. The central fiber carried the light from the 488 nm Argon laser to the tissue while the surrounding fibers collected the emitted fluorescence to the detector. When the fiber-optic microprobe was placed in the solutions containing various concentrations of fluorescent nanospheres (20 nm), either with or without 10% lipofundin as optical phantom, nanosphere concentration-dependent responses of the fluorescence intensity were observed. The microprobe was then implanted into the liver and the brain of anesthetized rats to monitor the in situ extravasation of pre-administered fluorescent nanospheres from vasculature following the ischemic insults. Both the hepatic and cerebral ischemic insults showed immediate increases of the extracellular 20 nm fluorescent nanospheres. The implantable fiber-optic microprobe constructed in present study provides itself as a minimally-invasive technique capable of investigating the vascular permeability for in vivo nanosphere delivery in both ischemic liver and brain.

Analysis of biological materials using a nuclear microprobe

NASA Astrophysics Data System (ADS)

Mulware, Stephen Juma

The use of nuclear microprobe techniques including: Particle induced x-ray emission (PIXE) and Rutherford backscattering spectrometry (RBS) for elemental analysis and quantitative elemental imaging of biological samples is especially useful in biological and biomedical research because of its high sensitivity for physiologically important trace elements or toxic heavy metals. The nuclear microprobe of the Ion Beam Modification and Analysis Laboratory (IBMAL) has been used to study the enhancement in metal uptake of two different plants. The roots of corn (Zea mays) have been analyzed to study the enhancement of iron uptake by adding Fe (II) or Fe(III) of different concentrations to the germinating medium of the seeds. The Fe uptake enhancement effect produced by lacing the germinating medium with carbon nanotubes has also been investigated. The aim of this investigation is to ensure not only high crop yield but also Fe-rich food products especially from calcareous soil which covers 30% of world's agricultural land. The result will help reduce iron deficiency anemia, which has been identified as the leading nutritional disorder especially in developing countries by the World Health Organization. For the second plant, Mexican marigold (Tagetes erecta ), the effect of an arbuscular mycorrhizal fungi (Glomus intraradices ) for the improvement of lead phytoremediation of lead contaminated soil has been investigated. Phytoremediation provides an environmentally safe technique of removing toxic heavy metals (like lead), which can find their way into human food, from lands contaminated by human activities like mining or by natural disasters like earthquakes. The roots of Mexican marigold have been analyzed to study the role of arbuscular mycorrhizal fungi in enhancement of lead uptake from the contaminated rhizosphere.

Geochemistry and origin of regional dolomites. Final report

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

Hanson, G.N.; Meyers, W.J.

1995-05-01

The main goal of our research on dolomites has been to better understand the composition of the fluids and processes of the fluid-rock interaction responsible for the formation of massive dolostones occurring over regional scales within sedimentary sequences. Understanding the timing of dolomitization, the fluids responsible for the dolomitization and the timing of the development of porosity has major economic ramifications in that dolomites are major oil reservoirs often having better reservoir properties than associated limestones. Our approach has been to apply trace element, major element, petrographic, crystallographic, stable isotope and radiogenic isotope systems to test models for the originsmore » of dolomites and to give information that may allow us to develop new models. Fluid compositions and processes are evaluated through the use of numerical models which we have developed showing the simultaneous evolution of the trace element and isotope systems during dolomitization. Our research has included the application of B, O, C, Sr, Nd and Pb isotope systematics and the trace elements Mn, Fe St, rare earth elements, Rb, Ba, U, Th, Pb, Zn, Na, Cl, F and SO{sub 4}{sup 2-}. Analyses are possible on individual cements or dolomite types using micro-sampling or microprobe techniques. The microprobe techniques used include synchrotron X-ray microprobe analysis at Brookhaven National Laboratory or electron microprobe at Stony Brook. Lack of a modern analogue for ancient massive dolostones has limited the application of the uniformitarian concept to developing models for the ancient regional dolostones. In addition it has not been possible to synthesize dolomite in the laboratory under conditions similar to the sedimentary or diagenetic possible environments in which the dolomites must have formed.« less

Scanning Auger Microprobe and atomic absorption studies of lunar volcanic volatiles

NASA Technical Reports Server (NTRS)

Cirlin, E. H.; Housley, R. M.

1979-01-01

Results on lunar volatile transport processes have been obtained by studying green and brown glass droplets, orange and black core tube samples and the surface sample 74241 with the Scanning Auger Microprobe (SAM) and by Flameless Atomic Absorption Analysis (FLAA). SAM analyses show that the most dominant volatiles in the top few atomic layers of droplets are Zn and S, confirming that the surface Zn and S are good indicators of pyroclastic origin, and they are not entirely present as ZnS. In addition, FLAA thermal release profiles show that almost all the Zn and Cd are on grain surfaces, indicating that Zn and Cd were completely outgassed from lava fountain products during the volcanic eruption, were recondensed during or after the eruptions, and are thus present as surface coating.

The Stanford-U.S. Geological Survey SHRIMP ion microprobe--a tool for micro-scale chemical and isotopic analysis

USGS Publications Warehouse

Bacon, Charles R.; Grove, Marty; Vazquez, Jorge A.; Coble, Matthew A.

2012-01-01

Answers to many questions in Earth science require chemical analysis of minute volumes of minerals, volcanic glass, or biological materials. Secondary Ion Mass Spectrometry (SIMS) is an extremely sensitive analytical method in which a 5–30 micrometer diameter "primary" beam of charged particles (ions) is focused on a region of a solid specimen to sputter secondary ions from 1–5 nanograms of the sample under high vacuum. The elemental abundances and isotopic ratios of these secondary ions are determined with a mass spectrometer. These results can be used for geochronology to determine the age of a region within a crystal thousands to billions of years old or to precisely measure trace abundances of chemical elements at concentrations as low as parts per billion. A partnership of the U.S. Geological Survey and the Stanford University School of Earth Sciences operates a large SIMS instrument, the Sensitive High-Resolution Ion Microprobe with Reverse Geometry (SHRIMP–RG) on the Stanford campus.

In situ ion-beam-induced luminescence analysis for evaluating a micrometer-scale radio-photoluminescence glass dosimeter

NASA Astrophysics Data System (ADS)

Kawabata, Shunsuke; Kada, Wataru; Parajuli, Raj Kumar; Matsubara, Yoshinori; Sakai, Makoto; Miura, Kenta; Satoh, Takahiro; Koka, Masashi; Yamada, Naoto; Kamiya, Tomihiro; Hanaizumi, Osamu

2016-06-01

Micrometer-scale responses of radio-photoluminescence (RPL) glass dosimeters to focused ionized particle radiation were evaluated by combining ion-beam-induced luminescence (IBIL) and proton beam writing (PBW) using a 3 MeV focused proton microbeam. RPL phosphate glass dosimeters doped with ionic Ag or Cu activators at concentrations of 0.2 and 0.1% were fabricated, and their scintillation intensities were evaluated by IBIL spectroscopy under a PBW micropatterning condition. Compared with the Ag-doped dosimeter, the Cu-doped dosimeter was more tolerant of the radiation, while the peak intensity of its luminescence was lower, under the precise dose control of the proton microprobe. Proton-irradiated areas were successfully recorded using these dosimeters and their RPL centers were visualized under 375 nm ultraviolet light. The reproduction of the irradiated region by post-RPL imaging suggests that precise estimation of irradiation dose using microdosimeters can be accomplished by optimizing RPL glass dosimeters for various proton microprobe applications in organic material analysis and in micrometer-scale material modifications.

Phase diagram and electrical behavior of silicon-rich iridium silicide compounds

NASA Technical Reports Server (NTRS)

Allevato, C. E.; Vining, Cronin B.

1992-01-01

The iridium-silicon phase diagram on the silicon-rich side was investigated by means of X-ray powder diffraction, density, differential thermal analysis, metalography, microprobe analysis, and electrical resistivity. Attempts were made to prepare eight previously reported silicon-rich iridium silicide compounds by arc melting and Bridgman-like growth. However, microprobe analysis identified only four distinct compositions: IrSi, Ir3Si4, Ir3Si5 and IrSi sub about 3. The existence of Ir4Si5 could not be confirmed in this study, even though the crystal structure has been previously reported. Differential thermal analysis (DTA) in conjunction with X-ray powder diffraction confirm polymorphism in IrSi sub about 3, determined to have orthorhombic and monoclinic unit cells in the high and low temperature forms. A eutectic composition alloy of 83 +/- 1 atomic percent silicon was observed between IrSi sub about 3 and silicon. Ir3Si4 exhibits distinct metallic behavior while Ir3Si5 is semiconducting. Both and IrSi and IrSi sub about 3 exhibit nearly temperature independent electrical resistivities on the order of 5-10 x 10 exp -6 ohms-m.

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

EPA Science Inventory

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

Core Community Specifications for Electron Microprobe Operating Systems: Software, Quality Control, and Data Management Issues

NASA Technical Reports Server (NTRS)

Fournelle, John; Carpenter, Paul

2006-01-01

Modem electron microprobe systems have become increasingly sophisticated. These systems utilize either UNIX or PC computer systems for measurement, automation, and data reduction. These systems have undergone major improvements in processing, storage, display, and communications, due to increased capabilities of hardware and software. Instrument specifications are typically utilized at the time of purchase and concentrate on hardware performance. The microanalysis community includes analysts, researchers, software developers, and manufacturers, who could benefit from exchange of ideas and the ultimate development of core community specifications (CCS) for hardware and software components of microprobe instrumentation and operating systems.

A thermal microprobe fabricated with wafer-stage processing

NASA Astrophysics Data System (ADS)

Zhang, Yongxia; Zhang, Yanwei; Blaser, Juliana; Sriram, T. S.; Enver, Ahsan; Marcus, R. B.

1998-05-01

A thermal microprobe has been designed and built for high resolution temperature sensing. The thermal sensor is a thin-film thermocouple junction at the tip of an atomic force microprobe (AFM) silicon probe needle. Only wafer-stage processing steps are used for the fabrication. For high resolution temperature sensing it is essential that the junction be confined to a short distance at the AFM tip. This confinement is achieved by a controlled photoresist coating process. Experiment prototypes have been made with an Au/Pd junction confined to within 0.5 μm of the tip, with the two metals separated elsewhere by a thin insulating oxide layer. Processing begins with double-polished, n-type, 4 in. diameter, 300-μm-thick silicon wafers. Atomically sharp probe tips are formed by a combination of dry and wet chemical etching, and oxidation sharpening. The metal layers are sputtering deposited and the cantilevers are released by a combination of KOH and dry etching. A resistively heated calibration device was made for temperature calibration of the thermal microprobe over the temperature range 25-110 °C. Over this range the thermal outputs of two microprobes are 4.5 and 5.6 μV/K and is linear. Thermal and topographical images are also obtained from a heated tungsten thin film fuse.

Fine-scale traverses in cumulate rocks, Stillwater Complex: A lunar analogue study

NASA Technical Reports Server (NTRS)

Elthon, Donald

1988-01-01

The objective was to document finite-scale compositional variations in cumulate rocks from the Stillwater Complex in Montana and to interpret these data in the context of planetary magma fractionation processes such as those operative during the formation of the Earth's Moon. This research problem involved collecting samples in the Stillwater Complex and analyzing them by electron microprobe, X-ray fluorescence (XRF), and instrumental neutron activation analysis (INAA). The electron microprobe is used to determine the compositions of cumulus and intercumulus phases in the rocks, the XRF is used to determine the bulk-rock major element and trace element (Y, Sr, Rb, Zr, Ni, and Cr) abundances, and the INAA lab. is used to determine the trace element (Sc, Co, Cr, Ni, Ta, Hf, U, Th, and the REE) abundances of mineral separates and bulk rocks.

Processing of copper converter slag for metals reclamation: Part II: mineralogical study.

PubMed

Deng, Tong; Ling, Yunhan

2004-10-01

Chemical and mineralogical characterizations of a copper converter slag, and its products obtained by curing with strong sulphuric acid and leaching with hot water, were carried out using ore microscopy, scanning electronic microscopy with energy dispersive spectrometry, wave-length dispersive X-ray fluorescence spectrometry, X-ray diffractometry and chemical phase analysis, which provided necessary information to develop a new process for treating such slag and further understanding of the chemical and mineralogical changes in the process.

Preparation and Thermoelectric Properties of Semiconcucting Zn(sub 4) Sb(sub 3)

NASA Technical Reports Server (NTRS)

Caillat, T.; Fleurial, J. P.; Barshchevsky, A.

1996-01-01

Hot-pressed samples fothe semiconducting compound Beta - Zn(sub 4) Sb(sub 3) were prepared and characterized by x-ray and microprobe analysis. Some physical properties of Beta - Zn(sub 4) Sb(sub 3) were determined and its thermoelectric properties measured between room temperature and 650K.

Synchrotron X-Ray Microprobe In-Situ Analysis of Extraterrestrial Particles Collected in Aerogel on the MIR Space Station

NASA Technical Reports Server (NTRS)

Flynn, G. J.; Sutton, S. R.; Horz, F.

2000-01-01

Using in-situ x-ray fluorescence, we determined the Cr/Fe, Mn/Fe and Ni/Fe of a particle captured in aerogel on MIR are approximately chondritic, indicating an extraterrestrial origin. Impurity of the aerogel precluded determining the Cu and Zn.

Examination of Laser Microprobe Vacuum Ultraviolet Ionization Mass Spectrometry with Application to Mapping Mars Returned Samples

NASA Astrophysics Data System (ADS)

Burton, A. S.; Berger, E. L.; Locke, D. R.; Lewis, E. K.; Moore, J. F.

2018-04-01

Laser microprobe of surfaces utilizing a two laser setup whereby the desorption laser threshold is lowered below ionization, and the resulting neutral plume is examined using 157nm Vacuum Ultraviolet laser light for mass spec surface mapping.

A study of GeV proton microprobe lens system designs with normal magnetic quadrupole

NASA Astrophysics Data System (ADS)

Dou, Yanxin; Jamieson, David N.; Liu, Jianli; Li, Liyi

2017-12-01

High energy proton irradiation has many applications to the study of radiation effects in semiconductor devices, biological tissues, proton tomography and space science. Many applications could be extended and enhanced by use of a high energy proton microprobe. However the design of a GeV proton microprobe must address significant challenges including beam collimation that minimizes ion scattering and the probe forming lens system for ions of high rigidity. Here we address the probe forming lens system design subject to several practical constraints including the use of non-superconducting normal magnetic quadrupole lenses, the ability to focus 1-5 GeV protons into 5 μm diameter microprobes and compatibility with the beam parameters of GeV proton accelerators. We show that 2, 3 and 4 lens systems of lenses with effective lengths up to 0.63 m can be employed for this purpose with a demagnification up to 58 and investigate the probe size limitations from beam brightness, lens aberrations and machining precision.

A microprobe for parallel optical and electrical recordings from single neurons in vivo.

PubMed

LeChasseur, Yoan; Dufour, Suzie; Lavertu, Guillaume; Bories, Cyril; Deschênes, Martin; Vallée, Réal; De Koninck, Yves

2011-04-01

Recording electrical activity from identified neurons in intact tissue is key to understanding their role in information processing. Recent fluorescence labeling techniques have opened new possibilities to combine electrophysiological recording with optical detection of individual neurons deep in brain tissue. For this purpose we developed dual-core fiberoptics-based microprobes, with an optical core to locally excite and collect fluorescence, and an electrolyte-filled hollow core for extracellular single unit electrophysiology. This design provides microprobes with tips < 10 μm, enabling analyses with single-cell optical resolution. We demonstrate combined electrical and optical detection of single fluorescent neurons in rats and mice. We combined electrical recordings and optical Ca²(+) measurements from single thalamic relay neurons in rats, and achieved detection and activation of single channelrhodopsin-expressing neurons in Thy1::ChR2-YFP transgenic mice. The microprobe expands possibilities for in vivo electrophysiological recording, providing parallel access to single-cell optical monitoring and control.

230Th-U dating of surficial deposits using the ion microprobe (SHRIMP-RG): A microstratigraphic perspective

USGS Publications Warehouse

Maher, K.; Wooden, J.L.; Paces, J.B.; Miller, D.M.

2007-01-01

We used the sensitive high-resolution ion microprobe reverse-geometry (SHRIMP-RG) to date pedogenic opal using the 230Th-U system. Due to the high-spatial resolution of an ion microprobe (typically 30 ??m), regions of pure opal within a sample can be targeted and detrital material can be avoided. In addition, because the technique is non-destructive, the sample can be preserved for other types of analyses including electron microprobe or other stable isotope or trace element ion microprobe measurements. The technique is limited to material with U concentrations greater than ???50 ppm. However, the high spatial resolution, small sample requirements, and the ability to avoid detrital material make this technique a suitable technique for dating many Pleistocene deposits formed in semi-arid environments. To determine the versatility of the method, samples from several different deposits were analyzed, including silica-rich pebble coatings from pedogenic carbonate horizons, a siliceous sinter deposit, and opaline silica deposited as a spring mound. U concentrations for 30-??m-diameter spots ranged from 50 to 1000 ppm in these types of materials. The 230Th/232Th activity ratios also ranged from ???100 to 106, eliminating the need for detrital Th corrections that reduce the precision of traditional U-Th ages for many milligram- and larger-sized samples. In pedogenic material, layers of high-U opal (ca. 500 ppm) are commonly juxtaposed next to layers of calcite with much lower U concentrations (1-2 ppm). If these types of samples are not analyzed using a technique with the appropriate spatial resolution, the ages may be strongly biased towards the age of the opal. Comparison with standard TIMS (Thermal Ionization Mass Spectrometry) measurements from separate microdrilled samples suggests that although the analytical precision of the ion microprobe (SHRIMP-RG) measurements is less than TIMS, the high spatial resolution results in better accuracy in the age determination for finely layered or complex deposits. The ion microprobe approach also may be useful for pre-screening samples to determine the age and degree of post-depositional alteration, analyzing finely layered samples or samples with complex growth histories, and obtaining simultaneous measurements of trace elements.

Installation and performance of the Budapest Hamburg proton microprobe

NASA Astrophysics Data System (ADS)

Kovács, I.; Kocsonya, A.; Kostka, P.; Szőkefalvi-Nagy, Z.; Schrang, K.; Krüger, A.; Niecke, M.

2005-04-01

A new scanning proton microprobe has been installed at the 5 MV Van de Graaff accelerator of the KFKI Research Institute for Particle and Nuclear Physics. It is the energy-upgraded version of the Hamburg proton microprobe dismantled in 2001. The probe forming system includes a pair of focusing quadrupoles and an additional quadrupole pair in front of it, which is applied to increase the proton beam divergence. The average probe size at 2.5 MeV proton energy is 2.2 μm × 1.1 μm. The test results on stability and the preliminary experiments on cement corrosion and fish otoliths are also presented.

High-speed microprobe for roughness measurements in high-aspect-ratio microstructures

NASA Astrophysics Data System (ADS)

Doering, Lutz; Brand, Uwe; Bütefisch, Sebastian; Ahbe, Thomas; Weimann, Thomas; Peiner, Erwin; Frank, Thomas

2017-03-01

Cantilever-type silicon microprobes with an integrated tip and a piezoresistive signal read out have successfully proven to bridge the gap between scanning force microscopy and stylus profilometry. Roughness measurements in high-aspect-ratio microstructures (HARMS) with depths down to 5 mm and widths down to 50 µm have been demonstrated. To improve the scanning speed up to 15 mm s-1, the wear of the tip has to be reduced. The atomic layer deposition (ALD) technique with alumina (Al2O3) has been tested for this purpose. Repeated wear measurements with coated and uncoated microprobe cantilevers have been carried out on a roughness standard at a speed of 15 mm s-1. The tip shape and the wear have been measured using a new probing tip reference standard containing rectangular silicon grooves with widths from 0.3 µm to 3 µm. The penetration depth of the microprobe allows one to measure the wear of the tip as well as the tip width and the opening angle of the tip. The roughness parameters obtained on the roughness standard during wear experiments agree well with the reference values measured with a calibrated stylus instrument, nevertheless a small amount of wear still is observable. Further research is necessary in order to obtain wear resistant microprobe tips for non-destructive inspection of microstructures in industry and microform measurements, for example in injection nozzles.

In-line metrology for roll-to-roll UV assisted nanoimprint lithography using diffractometry

NASA Astrophysics Data System (ADS)

Kreuzer, Martin; Whitworth, Guy L.; Francone, Achille; Gomis-Bresco, Jordi; Kehagias, Nikolaos; Sotomayor-Torres, Clivia M.

2018-05-01

We describe and discuss the optical design of a diffractometer to carry out in-line quality control during roll-to-roll nanoimprinting. The tool measures diffractograms in reflection geometry, through an aspheric lens to gain fast, non-invasive information of any changes to the critical dimensions of target grating structures. A stepwise tapered linear grating with constant period was fabricated in order to detect the variation in grating linewidth through diffractometry. The minimum feature change detected was ˜40 nm to a precision of 10 nm. The diffractometer was then integrated with a roll-to-roll UV assisted nanoimprint lithography machine to gain dynamic measurements in situ.

A versatile system for the rapid collection, handling and graphics analysis of multidimensional data

NASA Astrophysics Data System (ADS)

O'Brien, P. M.; Moloney, G.; O'Connor, A.; Legge, G. J. F.

1993-05-01

The aim of this work was to provide a versatile system for handling multiparameter data that may arise from a variety of experiments — nuclear, AMS, microprobe elemental analysis, 3D microtomography etc. Some of the most demanding requirements arise in the application of microprobes to quantitative elemental mapping and to microtomography. A system to handle data from such experiments had been under continuous development and use at MARC for the past 15 years. It has now been made adaptable to the needs of multiparameter (or single parameter) experiments in general. The original system has been rewritten, greatly expanded and made much more powerful and faster, by use of modern computer technology — a VME bus computer with a real time operating system and a RISC workstation running Unix and the X Window system. This provides the necessary (i) power, speed and versatility, (ii) expansion and updating capabilities (iii) standardisation and adaptability, (iv) coherent modular programming structures, (v) ability to interface to other programs and (vi) transparent operation with several levels, involving the use of menus, programmed function keys and powerful macro programming facilities.

MICROCHARACTERIZATION OF ARSENIC- AND SELENIUM-BEARING PYRITE IN UPPER FREEPORT COAL, INDIANA COUNTY, PENNSYLVANIA.

USGS Publications Warehouse

Minkin, J.A.; Finkelman, R.B.; Thompson, C.L.; Chao, E.C.T.; Ruppert, L.F.; Blank, H.; Cecil, C.B.

1984-01-01

Optical and scanning electron microscope as well as electron and proton microprobe techniques have been used in a detailed investigation of the modes of occurrence of arsenic and selenium in pyrite in Upper Freeport coal from the Homer City area, Indiana County, Pennsylvania. Polished blocks were prepared from columnar samples of the coal bed to represent particular zones continuously from top to bottom. Initial selection of zones to be studied was based on chemical analysis of bench-channel samples. Microprobe data indicate that the highest concentrations of arsenic (as great as 1. 5 wt. %) are apparently in solid solution in pyrite within a limited stratigraphic interval of the coal bed. Smaller amounts of arsenic and selenium (concentrations up to approximately 0. 1 and 0. 2 wt. % respectively) were detected at isolated points within pyrite grains in various strata of the coal bed.

Nuclear microprobe imaging of gallium nitrate in cancer cells

NASA Astrophysics Data System (ADS)

Ortega, Richard; Suda, Asami; Devès, Guillaume

2003-09-01

Gallium nitrate is used in clinical oncology as treatment for hypercalcemia and for cancer that has spread to the bone. Its mechanism of antitumor action has not been fully elucidated yet. The knowledge of the intracellular distribution of anticancer drugs is of particular interest in oncology to better understand their cellular pharmacology. In addition, most metal-based anticancer compounds interact with endogenous trace elements in cells, altering their metabolism. The purpose of this experiment was to examine, by use of nuclear microprobe analysis, the cellular distribution of gallium and endogenous trace elements within cancer cells exposed to gallium nitrate. In a majority of cellular analyses, gallium was found homogeneously distributed in cells following the distribution of carbon. In a smaller number of cells, however, gallium appeared concentrated together with P, Ca and Fe within round structures of about 2-5 μm diameter located in the perinuclear region. These intracellular structures are typical of lysosomial material.

Volatility in the lunar crust: Trace element analyses of lunar minerals by PIXE proton microprobe

NASA Technical Reports Server (NTRS)

Norman, M. D.; Griffin, W. L.; Ryan, C. G.

1993-01-01

In situ determination of mineral compositions using microbeam techniques can characterize magma compositions through mineral-melt partitioning, and be used to investigate fine-grained or rare phases which cannot be extracted for analysis. Abundances of Fe, Mn, Sr, Ga, Zr, Y, Nb, Zn, Cu, Ni, Se, and Sb were determined for various mineral phases in a small number of lunar highlands rocks using the PIXE proton microprobe. Sr/Ga ratios of plagioclase and Mn/Zn ratios of mafic silicates show that the ferroan anorthosites and Mg-suite cumulates are depleted in volatile lithophile elements to about the same degree compared with chondrites and the Earth. This links the entire lunar crust to common processes or source compositions. In contrast, secondary sulfides in Descartes breccia clasts are enriched in chalcophile elements such as Cu, Zn, Ni, Se, and Sb, and represent a potential resource in the lunar highlands.

Silver and mercury in single gold grains from the Witwatersrand and Barberton, South Africa

NASA Astrophysics Data System (ADS)

von Gehlen, K.

1983-10-01

The contents of silver and mercury in 323 spots on gold grains from seven localities of the Witwatersrand palaeo-placer and Archaean vein deposits from Barberton were measured using an electron microprobe. The objective was to obtain information on the extent of gold alteration during fluvial transport and post-depositional geological processes. The results, however, show that Ag and Hg are distributed homogeneously in the gold grains studied. No indications were found that the gold was transported in solution nor that leaching took place in an oxidizing fluvial environment. This strongly suggests that the Ag and Hg contents in Witwatersrand gold grains represent geochemical ‘fingerprints’ inherited from their eroded primary sources. Combined analysis for Ag and Hg in Witwatersrand gold grains by electron microprobe can therefore be a valuable tool in establishing the types of primary sources for the gold.

CAMECA IMS 1300-HR3: The New Generation Ion Microprobe

NASA Astrophysics Data System (ADS)

Peres, P.; Choi, S. Y.; Renaud, L.; Saliot, P.; Larson, D. J.

2016-12-01

The success of secondary ion mass spectrometry (SIMS) in Geo- and Cosmo-chemistry relies on its performance in terms of: 1) very high sensitivity (mandatory for high precision measurements or to achieve low detection limits); 2) a broad mass range of elemental and isotopic species, from low mass (H) to high mass (U and above); 3) in-situ analysis of any solid flat polished surface; and 4) high spatial resolution from tens of microns down to sub-micron scale. The IMS 1300-HR3 (High Reproducibility, High spatial Resolution, High mass Resolution) is the latest generation of CAMECA's large geometry magnetic sector SIMS (or ion microprobe), successor to the internationally recognized IMS 1280-HR. The 1300-HR3delivers unmatched analytical performance for a wide range of applications (stable isotopes, geochronology, trace elements, nuclear safeguards and environmental studies…) due to: • High brightness RF-plasma oxygen ion source with enhanced beam density and current stability, dramatically improving spatial resolution, data reproducibility, and throughput • Automated sample loading system with motorized sample height (Z) adjustment, significantly increasing analysis precision, ease-of-use, and productivity • UV-light microscope for enhanced optical image resolution, together with dedicated software for easy sample navigation (developed by University of Wisconsin, USA) • Low noise 1012Ω resistor Faraday cup preamplifier boards for measuring low signal intensities In addition, improvements in electronics and software have been integrated into the new instrument. In order to meet a growing demand from geochronologists, CAMECA also introduces the KLEORA, which is a fully optimized ion microprobe for advanced mineral dating derived from the IMS 1300-HR3. Instrumental developments as well as data obtained for stable isotope and U-Pb dating applications will be presented in detail.

Scanning ion images; analysis of pharmaceutical drugs at organelle levels

NASA Astrophysics Data System (ADS)

Larras-Regard, E.; Mony, M.-C.

1995-05-01

With the ion analyser IMS 4F used in microprobe mode, it is possible to obtain images of fields of 10 × 10 [mu]m2, corresponding to an effective magnification of 7000 with lateral resolution of 250 nm, technical characteristics that are appropriate for the size of cell organelles. It is possible to characterize organelles by their relative CN-, P- and S- intensities when the tissues are prepared by freeze fixation and freeze substitution. The recognition of organelles enables correlation of the tissue distribution of ebselen, a pharmaceutical drug containing selenium. The various metabolites characterized in plasma, bile and urine during biotransformation of ebselen all contain selenium, so the presence of the drug and its metabolites can be followed by images of Se. We were also able to detect the endogenous content of Se in tissue, due to the increased sensitivity of ion analysis in microprobe mode. Our results show a natural occurrence of Se in the border corresponding to the basal lamina of cells of proximal but not distal tubules of the kidney. After treatment of rats with ebselen, an additional site of Se is found in the lysosomes. We suggest that in addition to direct elimination of ebselen and its metabolites by glomerular filtration and urinary elimination, a second process of elimination may occur: Se compounds reaching the epithelial cells via the basal lamina accumulate in lysosomes prior to excretion into the tubular fluid. The technical developments of using the IMS 4F instrument in the microprobe mode and the improvement in preparation of samples by freeze fixation and substitution further extend the limit of ion analysis in biology. Direct imaging of trace elements and molecules marked with a tracer make it possible to determine their targets by comparison with images of subcellular structures. This is a promising advance in the study of pathways of compounds within tissues, cells and the whole organism.

The relationship between crystal structure and methyl and t-butyl group dynamics in van der Waals organic solids

NASA Astrophysics Data System (ADS)

Beckmann, Peter A.; Paty, Carol; Allocco, Elizabeth; Herd, Maria; Kuranz, Carolyn; Rheingold, Arnold L.

2004-03-01

We report x-ray diffractometry in a single crystal of 2-t-butyl-4-methylphenol (TMP) and low-frequency solid state nuclear magnetic resonance (NMR) proton relaxometry in a polycrystalline sample of TMP. The x-ray data show TMP to have a monoclinic, P21/c, structure with eight molecules per unit cell and two crystallographically inequivalent t-butyl group (C(CH3)3) sites. The proton spin-lattice relaxation rates were measured between 90 and 310 K at NMR frequencies of 8.50, 22.5, and 53.0 MHz. The relaxometry data is fitted with two models characterizing the dynamics of the t-butyl groups and their constituent methyl groups, both of which are consistent with the determined x-ray structure. In addition to presenting results for TMP, we review previously reported x-ray diffractometry and low-frequency NMR relaxometry in two other van der Waals solids which have a simpler structure. In both cases, a unique model for the reorientational dynamics was found. Finally, we review a similar previously reported analysis in a van der Waals solid with a very complex structure in which case fitting the NMR relaxometry requires very many parameters and serves mainly as a flag for a careful x-ray diffraction study.

Electron microprobe study of lunar and planetary zoned plagioclase feldspars: An analytical and experimental study of zoning in plagioclase

NASA Technical Reports Server (NTRS)

Smith, R. K.; Lofgren, G. E.

1982-01-01

Natural and experimentally grown zoned plagioclase feldspars were examined by electron microprobe. The analyses revealed discontinuous, sector, and oscillary chemical zoning superimposed on continuous normal or reverse zoning trends. Postulated mechanisms for the origin of zoning are based on either physical changes external to the magma (P, T, H2O saturation) or kinetic changes internal to the magma (diffusion, supersaturation, growth rate). Comparison of microprobe data on natural zoned plagioclase with zoned plagioclase grown in controlled experiments show that it may be possible to distinguish zonal development resulting from physio-chemical changes to the bulk magma from local kinetic control on the growth of individual crystals.

Focused Heavy Ion Nuclear Microprobe facility at the University of North Texas

NASA Astrophysics Data System (ADS)

Guo, B. N.; Yang, C.; El Bouanani, M.; Duggan, J. L.; McDaniel, F. D.

1999-10-01

A Focused Heavy Ion Nuclear Microprobe facility has been constructed at the University of North Texas. The microprobe utilizes two separated Russian magnetic quadrupole quadruplets. The two identical magnetic quadrupole doublet lenses are separated by 2.61 meters. The lens system with ~ 80 times demagnification has the ability to focus proton, alpha particle, or heavier ions down to a spot size of ~ 1 μm. The microprobe components rest on a 7 meter steel beam support with vibration isolation. A computer provides control for the lens power supplies and also the parameters for a post-lens scanning coil to raster-scan the beam across the sample. Up to four detection channels can be used for simultaneous data acquisition under VME control. A RISC workstation is used to collect, display and analyze the data. The data is transferred via ethernet. A detailed description of the facility and data acquisition system along with preliminary testing results on TEM grids with Rutherford Backscattering Spectrometry and the Ion Beam Induced Charge Collection techniques will be presented.

Biological Effects of Laser Radiation. Volume I. Review of the Literature on Biological Effects of Laser Radiation-to 1965.

DTIC Science & Technology

1978-10-17

because of the rapid progress made in laser technology to date. The use of the Laser Microprobe in spectrochemical analysis of the elements is based on...spectroscopy to vaporize microscopic amounts of samples for elemental analysis . On the other hand, the intense, highly monochromatic laser beam is being...employed as a light source for Raman spectroscopy to study molecular structure. These two uses of lasers in spectroscopic analysis have been sucessful

Laser-Ablation (U-Th)/He Geochronology

NASA Astrophysics Data System (ADS)

Hodges, K.; Boyce, J.

2003-12-01

Over the past decade, ultraviolet laser microprobes have revolutionized the field of 40Ar/39Ar geochronology. They provide unprecedented information about Ar isotopic zoning in natural crystals, permit high-resolution characterization of Ar diffusion profiles produced during laboratory experiments, and enable targeted dating of multiple generations of minerals in thin section. We have modified the analytical protocols used for 40Ar/39Ar laser microanalysis for use in (U-Th)/He geochronologic studies. Part of the success of the 40Ar/39Ar laser microprobe stems from fact that measurements of Ar isotopic ratios alone are sufficient for the calculation of a date. In contrast, the (U-Th)/He method requires separate analysis of U+Th and 4He. Our method employs two separate laser microprobes for this process. A target mineral grain is placed in an ultrahigh vacuum chamber fitted with a window of appropriate composition to transmit ultraviolet radiation. A focused ArF (193 nm) excimer laser is used to ablate tapered cylindrical pits on the surface of the target. The liberated material is scrubbed with a series of getters in a fashion similar to that used for 40Ar/39Ar geochronology, and the 4He abundance is determined using a quadrupole mass spectrometer with well-calibrated sensitivity. A key requirement for calculation of the 4He abundance in the target is a precise knowledge of the volume of the ablation pit. This is the principal reason why we employ the ArF excimer for 4He analysis rather than a less-expensive frequency-multiplied Nd-YAG laser; the excimer creates tapered cylindrical pits with extremely reproducible and easily characterized geometry. After 4He analysis, U and Th are measured on the same sample surface using the more familiar technique of laser-ablation inductively coupled plasma mass spectrometry (LA-ICPMS). Our early experiments have been done using a frequency-quintupled Nd-YAG microprobe (213nm), While the need to analyze U+Th and He in separate ablation experiments results in considerably worse spatial resolution than that typically possible for 40Ar/39Ar laser microprobe dating, it is possible to site the LA-ICPMS ablation pit within a few microns of the pit used for He extraction, or to simply re-occupy and enlarge the original ablation pit. The potential effective spatial resolution of the technique is thus on the order of a few tens to roughly 100 microns. As a proof-of-concept exercise, we have applied this technique to fluorapatite from Cerro de Mercado, Durango, Mexico, which has a generally accepted (U-Th)/He age of 32.1 +/- 3.4 Ma (2 sigma) based on single-crystal fusion analyses reported by House et al. (2000, EPSL). Using the approach described above, we made 48 separate age measurements on a 12 mm polished section cut through a single crystal of Durango fluorapatite perpendicular to its c axis. The measured dates yield a mean of 34.9 +/- 5.1 Ma (2 sigma), with a total dispersion of dates comparable to that reported by House et al. Much of the apparent age variation observed in both studies is due to documented U+Th heterogeneities in single crystals of the Durango fluorapatite. Nevertheless, the consistency of the laser ablation and conventional results for this material is striking. Compared to conventional laser and furnace methods of (U-Th)/He geochronology, the laser microprobe approach offers substantially improved spatial resolution, and the ability to avoid (or at least minimize) alpha-ejection corrections. In addition, the method affords improved sample throughput, such that age estimates for homogeneous materials can be made with considerably higher precision based on a larger number of analyses.

Defense Small Business Innovation Research Program (SBIR). Abstracts of Phase I Awards. 1986.

DTIC Science & Technology

1986-01-01

RELATIVE HUMIDITY AT TEMPERATURES FOUND IN ARCTIC ENVIRONMENTS. IT IS BASED ON THE OBSERVATION THAT CERTAIN FLUORESCENT AND PHOSPHORESCENT COMPOUNDS ...FREEDMAN TITLE: III-V COMPOUNDS TRACE ELEMENT PROFILE ANALYSIS USING LASER ASSISTED S PECTROSCOPY T 55 OFFICE: RADC/DOR A NOVEL MICROPROBE ANALYSIS...AND II-VI AND III-V COMPOUNDS . THESE ADVANTAGES MAKE THE LSCE TECHNIQUE PARTICULARY WELL SUITED TO THE DEPOSITION OF QUANTUM WELL AND SUPERLATT ICE

X-ray microprobe analysis of platelets. Principles, methods and review of the literature.

PubMed

Yarom, R

1983-01-01

Platelets are well suited to X-ray microanalysis as there is no need for chemical fixation or sectioning, and the concentrations of calcium and phosphorus are above 10(-3). The principles of the technique, the methods of specimen preparation, instrumental conditions during analysis and ways of quantitation are described. This is followed by a review of published reports and a brief summary of the author's own work in the field.

Study of Italian Renaissance sculptures using an external beam nuclear microprobe

NASA Astrophysics Data System (ADS)

Zucchiatti, A.; Bouquillon, A.; Moignard, B.; Salomon, J.; Gaborit, J. R.

2000-03-01

The use of an extracted proton micro-beam for the PIXE analysis of glazes is discussed in the context of the growing interest in the creation of an analytical database on Italian Renaissance glazed terracotta sculptures. Some results concerning the frieze of an altarpiece of the Louvre museum, featuring white angels and cherubs heads, are presented.

Determination of nitrogen in coal macerals using electron microprobe technique-experimental procedure

USGS Publications Warehouse

Mastalerz, Maria; Gurba, L.W.

2001-01-01

This paper discusses nitrogen determination with the Cameca SX50 electron microprobe using PCO as an analyzing crystal. A set of conditions using differing accelerating voltages, beam currents, beam sizes, and counting times were tested to determine parameters that would give the most reliable nitrogen determination. The results suggest that, for the instrumentation used, 10 kV, current 20 nA, and a counting time of 20 s provides the most reliable nitrogen determination, with a much lower detection limit than the typical concentration of this element in coal. The study demonstrates that the electron microprobe technique can be used to determine the nitrogen content of coal macerals successfully and accurately. ?? 2001 Elsevier Science B.V. All rights reserved.

Characterization of Alq3 thin films by a near-field microwave microprobe.

PubMed

Hovsepyan, Artur; Lee, Huneung; Sargsyan, Tigran; Melikyan, Harutyun; Yoon, Youngwoon; Babajanyan, Arsen; Friedman, Barry; Lee, Kiejin

2008-09-01

We observed tris-8-hydroxyquinoline aluminum (Alq3) thin films dependence on substrate heating temperatures by using a near-field microwave microprobe (NFMM) and by optical absorption at wavelengths between 200 and 900 nm. The changes of absorption intensity at different substrate heating temperatures are correlated to the changes in the sheet resistance of Alq3 thin films.

Examination of Surveyor 3 parts with the scanning electron microscope and electron microprobe

NASA Technical Reports Server (NTRS)

Chodos, A. A.; Devaney, J. R.; Evens, K. C.

1972-01-01

Two screws and two washers, several small chips of tubing, and a fiber removed from a third screw were examined with the scanning electron microscope and the electron microprobe. The purpose of the examination was to determine the nature of the material on the surface of these samples and to search for the presence of meteoritic material.

A Comparison of Microstructure and Properties of Equivalent Strength Ingot Metallurgy and Powder Metallurgy 7XXX Aluminum Alloys.

DTIC Science & Technology

1981-08-01

electron microprobe analysis and other laboratory procedures is also acknowledged. The author recognizes the considerable contributions of Ms. Cheryl ...J. Knott , Acta Met., 23, (7), (1975), 841. 473. A. Tetelman and A. McEvily, op. cit. 474. J. Feeney and J. McMillan and R. Wei, Met. Trans., 1, (1970

In situ study of the growth and degradation processes in tetragonal lysozyme crystals on a silicon substrate by high-resolution X-ray diffractometry

NASA Astrophysics Data System (ADS)

Kovalchuk, M. V.; Prosekov, P. A.; Marchenkova, M. A.; Blagov, A. E.; D'yakova, Yu. A.; Tereshchenko, E. Yu.; Pisarevskii, Yu. V.; Kondratev, O. A.

2014-09-01

The results of an in situ study of the growth of tetragonal lysozyme crystals by high-resolution X-ray diffractometry are considered. The crystals are grown by the sitting-drop method on crystalline silicon substrates of different types: both on smooth substrates and substrates with artificial surface-relief structures using graphoepitaxy. The crystals are grown in a special hermetically closed crystallization cell, which enables one to obtain images with an optical microscope and perform in situ X-ray diffraction studies in the course of crystal growth. Measurements for lysozyme crystals were carried out in different stages of the crystallization process, including crystal nucleation and growth, developed crystals, the degradation of the crystal structure, and complete destruction.

Physical properties of organic particulate UV-absorbers used in sunscreens. I. Determination of particle size with fiber-optic quasi-elastic light scattering (FOQELS), disc centrifugation, and laser diffractometry.

PubMed

Herzog, Bernd; Katzenstein, Armin; Quass, Katja; Stehlin, Albert; Luther, Helmut

2004-03-01

In this study microparticles consisting of a benzotriazole derivative, which are used as absorbers for UV radiation in cosmetic sunscreens, were investigated. The particles were micronized in presence of a dispersing agent by means of a ball milling process. According to the energy input different particle sizes were produced in the range of 0.16 to 4 microm. The particle sizes obtained after different stages of the micronization process were measured using fiber-optic quasi-elastic light scattering (FOQELS), disc centrifugation, and laser diffractometry. All methods showed satisfactory agreement over the whole range of sizes. With the FOQELS technique the particle size distribution could be resolved to sizes well below 0.1 microm.

The elemental move characteristic of nickel-based alloy in molten salt corrosion by using nuclear microprobe

NASA Astrophysics Data System (ADS)

Lei, Qiantao; Liu, Ke; Gao, Jie; Li, Xiaolin; Shen, Hao; Li, Yan

2017-08-01

Nickel-based alloys as candidate materials for Thorium Molten Salt Reactor (TMSR), need to be used under high temperature in molten salt environment. In order to ensure the safety of the reactor running, it is necessary to study the elemental move characteristic of nickel-based alloys in the high temperature molten salts. In this work, the scanning nuclear microprobe at Fudan University was applied to study the elemental move. The Nickel-based alloy samples were corroded by molten salt at different temperatures. The element concentrations in the Nickel-based alloys samples were determined by the scanning nuclear microprobe. Micro-PIXE results showed that the element concentrations changed from the interior to the exterior of the alloy samples after the corrosion.

Laser-excited fluorescence of rare earth elements in fluorite: Initial observations with a laser Raman microprobe

USGS Publications Warehouse

Burruss, R.C.; Ging, T.G.; Eppinger, R.G.; Samson, a.M.

1992-01-01

Fluorescence emission spectra of three samples of fluorite containing 226-867 ppm total rare earth elements (REE) were excited by visible and ultraviolet wavelength lines of an argon ion laser and recorded with a Raman microprobe spectrometer system. Narrow emission lines ( 0.9 for Eu2+ and 0.99 for Er3+. Detection limits for three micrometer spots are about 0.01 ppm Eu2+ and 0.07 ppm Er3+. These limits are less than chondrite abundance for Eu and Er, demonstrating the potential microprobe analytical applications of laser-excited fluorescence of REE in fluorite. However, application of this technique to common rock-forming minerals may be hampered by competition between fluorescence emission and radiationless energy transfer processes involving lattice phonons. ?? 1992.

The grape cluster, metal particle 63344,1. [in lunar coarse fines

NASA Technical Reports Server (NTRS)

Goldstein, J. I.; Axon, H. J.; Agrell, S. O.

1975-01-01

The grape cluster metal particle 63344,1 found in lunar coarse fines is examined using the scanning electron microscope (SEM), electron microprobe, and an optical microscope. This metal particle is approximately 0.5 cm in its largest dimension and consists of hundreds of metallic globules welded together to form a structure somewhat like a bunch of grapes. Electron microprobe analysis for Fe, Ni, Co, P, and S in the metal was carried out using wavelength dispersive detectors. No primary solidification structure is observed in the globules, and the particle is slow cooled from the solidification temperature (nearly 1300 C) taking days to probably months to reach 600 C. Two mechanisms for the formation of globules are proposed. One mechanism involves the primary impact of an iron meteorite which produces a metallic liquid and vapor phase. The second mechanism involves the formation of a liquid pool of metal after impact of an iron meteorite projectile followed by a secondary impact in the liquid metal pool.

Experimental determination of the partitioning of gallium between solid iron metal and synthetic basaltic melt Electron and ion microprobe study

NASA Technical Reports Server (NTRS)

Drake, M. J.; Newsom, H. E.; Reed, S. J. B.; Enright, M. C.

1984-01-01

The distribution of Ga between solid Fe metal and synthetic basaltic melt is investigated experimentally at temperatures of 1190 and 1330 C, and over a narrow range of oxygen fugacities. Metal-silicate reversal experiments were conducted, indicating a close approach to equilibrium. The analysis of the partitioned products was performed using electron and ion microprobes. At one bar total pressure, the solid metal/silicate melt partition coefficient D(Ga) is used to evaluate metal-silicate fractionation processes in the earth, moon, and Eucrite Parent Body (EPB). It is found that the depletion of Ga abundances in the EPB is due to the extraction of Ga into a metallic core. Likewise, the depletion of Ga in the lunar mantle is consistent with the extraction of Ga into a smaller lunar core if Ga was originally present in a subchondritic concentration. The relatively high Ga abundances in the earth's mantle are discussed, with reference to several theoretical models.

Development of an external beam nuclear microprobe on the Aglae facility of the Louvre museum

NASA Astrophysics Data System (ADS)

Calligaro, T.; Dran, J.-C.; Ioannidou, E.; Moignard, B.; Pichon, L.; Salomon, J.

2000-03-01

The external beam line of our facility has been recently equipped with the focusing system previously mounted on a classical nuclear microprobe. When using a 0.1 μm thick Si 3N 4 foil for the exit window and flowing helium on the sample under analysis, a beam spot as small as 10 μm is attainable at a distance of 3 mm from the window. Elemental micromapping is performed by mechanical scanning. An electronic device has been designed which allows XY scanning by moving the sample under the beam by steps down to 0.1 μm. Beam monitoring is carried out by means of the weak X-ray signal emitted by the exit foil and detected by a specially designed Si(Li) detector cooled by Peltier effect. The characteristics of external beams of protons and alpha particles are evaluated by means of resonance scanning and elemental mapping of a grid. An example of application is presented, dealing with elemental micro-mapping of inclusions in gemstones.

A novel analytical method for pharmaceutical polymorphs by terahertz spectroscopy and the optimization of crystal form at the discovery stage.

PubMed

Ikeda, Yukihiro; Ishihara, Yoko; Moriwaki, Toshiya; Kato, Eiji; Terada, Katsuhide

2010-01-01

A novel analytical method for the determination of pharmaceutical polymorphs was developed using terahertz spectroscopy. It was found out that each polymorph of a substance showed a specific terahertz absorption spectrum. In particular, analysis of the second derivative spectrum was enormously beneficial in the discrimination of closely related polymorphs that were difficult to discern by powder X-ray diffractometry. Crystal forms that were obtained by crystallization from various solvents and stored under various conditions were specifically characterized by the second derivative of each terahertz spectrum. Fractional polymorphic transformation for substances stored under stressed conditions was also identified by terahertz spectroscopy during solid-state stability test, but could not be detected by powder X-ray diffractometry. Since polymorphs could be characterized clearly by terahertz spectroscopy, further physicochemical studies could be conducted in a timely manner. The development form of compound examined was determined by the results of comprehensive physicochemical studies that included thermodynamic relationships, as well as chemical and physicochemical stability. In conclusion, terahertz spectroscopy, which has unique power in the elucidation of molecular interaction within a crystal lattice, can play more important role in physicochemical research. Terahertz spectroscopy has a great potential as a tool for polymorphic determination, particularly since the second derivative of the terahertz spectrum possesses high sensitivity for pharmaceutical polymorphs.

Influence of Bulk Chemical Composition on Relative Sensitivity Factors for 55Mn/52Cr by SIMS: Implications for the 53Mn-53Cr Chronometer

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

Matzel, J; Jacobsen, B; Hutcheon, I D

2009-09-09

The {sup 53}Mn-{sup 53}Cr systematics of meteorite samples provide an important high resolution chronometer for early solar system events. Accurate determination of the initial abundance of {sup 53}Mn ({tau}{sub 1/2} = 3.7 Ma) by secondary ion mass spectrometry (SIMS) is dependent on properly correcting for differing ion yields between Mn and Cr by use of a relative sensitivity factor (RSF). Ideal standards for SIMS analysis should be compositionally and structurally similar to the sample of interest. However, previously published Mn-Cr studies rely on few standards (e.g., San Carlos olivine, NIST 610 glass) despite significant variations in chemical composition. We investigatemore » a potential correlation between RSF and bulk chemical composition by determining RSFs for {sup 55}Mn/{sup 52}Cr in 11 silicate glass and mineral standards (San Carlos olivine, Mainz glasses KL2-G, ML3B-G, StHs6/80-G, GOR128-G, BM90/21-G, and T1-G, NIST 610 glass, and three LLNL pyroxene-composition glasses). All standards were measured on the Cameca ims-3f ion microprobe at LLNL, and a subset were also measured on the Cameca ims-1270 ion microprobe at the Geological Survey of Japan. The standards cover a range of bulk chemical compositions with SiO{sub 2} contents of 40-71 wt.%, FeO contents of 0.05-20 wt.% and Mn/Cr ratios between 0.4 and 58. We obtained RSF values ranging from 0.83 to 1.15. The data obtained on the ims-1270 ion microprobe are within {approx}10% of the RSF values obtained on the ims-3f ion microprobe, and the RSF determined for San Carlos olivine (0.86) is in good agreement with previously published data. The typical approach to calculating an RSF from multiple standard measurements involves making a linear fit to measured {sup 55}Mn/{sup 52}Cr versus true {sup 55}Mn/{sup 52}Cr. This approach may be satisfactory for materials of similar composition, but fails when compositions vary significantly. This is best illustrated by the {approx}30% change in RSF we see between glasses with similar Mn/Cr ratios but variable Fe and Na content. We are developing an approach that uses multivariate analysis to evaluate the importance of different chemical components in controlling the RSF and predict the RSF of unknowns when standards of appropriate composition are not available. Our analysis suggests that Fe, Si, and Na are key compositional factors in these silicate standards. The RSF is positively correlated with Fe and Si and negatively correlated with Na. Work is currently underway to extend this analysis to a wider range of chemical compositions and to evaluate the variability of RSF on measurements obtained by NanoSIMS.« less

Fused Bead Analysis of Diogenite Meteorites

NASA Technical Reports Server (NTRS)

Mittlefehldt, D.W.; Beck, B.W.; McSween, H.Y.; Lee, C.T. A.

2009-01-01

Bulk rock chemistry is an essential dataset in meteoritics and planetary science [1]. A common method used to obtain the bulk chemistry of meteorites is ICP-MS. While the accuracy, precision and low detection limits of this process are advantageous [2], the sample size used for analysis (approx.70 mg) can be a problem in a field where small and finite samples are the norm. Fused bead analysis is another bulk rock analytical technique that has been used in meteoritics [3]. This technique involves forming a glass bead from 10 mg of sample and measuring its chemistry using a defocused beam on a microprobe. Though the ICP-MS has lower detection limits than the microprobe, the fused bead method destroys a much smaller sample of the meteorite. Fused bead analysis was initially designed for samples with near-eutectic compositions and low viscosities. Melts generated of this type homogenize at relatively low temperatures and produce primary melts near the sample s bulk composition [3]. The application of fused bead analysis to samples with noneutectic melt compositions has not been validated. The purpose of this study is to test if fused bead analysis can accurately determine the bulk rock chemistry of non-eutectic melt composition meteorites. To determine this, we conduct two examinations of the fused bead. First, we compare ICP-MS and fused bead results of the same samples using statistical analysis. Secondly, we inspect the beads for the presence of crystals and chemical heterogeneity. The presence of either of these would indicate incomplete melting and quenching of the bead.

Growth, structural, optical, thermal and mechanical properties of ammonium pentaborate single crystal.

PubMed

Balakrishnan, T; Bhagavannarayana, G; Ramamurthi, K

2008-11-15

Nonlinear optical single crystals of ammonium pentaborate (APB) were grown by the slow cooling method from aqueous solution. Grown crystal was characterized by powder X-ray diffraction (PXRD) and FT-IR spectral analysis. Perfection of the grown crystal was evaluated by high-resolution X-ray diffractometry (HRXRD). The effect of nylon threading on the perfection of the grown bigger crystal was also studied by HRXRD. The range and percentage of optical transmission was ascertained by recording UV-vis-NIR spectrum. Thermal properties were investigated by TG-DTA and DSC analyses. Its mechanical hardness was estimated by Vickers microhardness tester.

Micro-PIXE analysis of silicate reference standards

USGS Publications Warehouse

Czamanske, G.K.; Sisson, T.W.; Campbell, J.L.; Teesdale, W.J.

1993-01-01

The accuracy and precision of the University of Guelph proton microprobe have been evaluated through trace-element analysis of well-characterized silicate glasses and minerals, including BHVO-1 glass, Kakanui augite and hornblende, and ten other natural samples of volcanic glass, amphibole, pyroxene, and garnet. Using the 2.39 wt% Mo in a NIST steel as the standard, excellent precision and agreement between reported and analyzed abundances were obtained for Fe, Ni, Cu, Zn, Ga, Rb, Sr, Y, Zr, and Nb. -from Authors

Optically continuous silcrete quartz cements of the St. Peter Sandstone: High precision oxygen isotope analysis by ion microprobe

NASA Astrophysics Data System (ADS)

Kelly, Jacque L.; Fu, Bin; Kita, Noriko T.; Valley, John W.

2007-08-01

A detailed oxygen isotope study of detrital quartz and authigenic quartz overgrowths from shallowly buried (<1 km) quartz arenites of the St. Peter Sandstone (in SW Wisconsin) constrains temperature and fluid sources during diagenesis. Quartz overgrowths are syntaxial (optically continuous) and show complex luminescent zonation by cathodoluminescence. Detrital quartz grains were separated from 53 rocks and analyzed for oxygen isotope ratio by laser fluorination, resulting in an average δ 18O of 10.0 ± 0.2‰ (1SD, n = 109). Twelve thin sections were analyzed by CAMECA-1280 ion microprobe (6-10 μm spot size, analytical precision better than ±0.2‰, 1SD). Detrital quartz grains have an average δ 18O of 10.0 ± 1.4‰ (1SD, n = 91) identical to the data obtained by laser fluorination. The ion microprobe data reveal true variability that is otherwise lost by homogenization of powdered samples necessary for laser fluorination. Laser fluorination uses samples that are one million times larger than the ion microprobe. Whole rock (WR) samples from the 53 rocks were analyzed by laser fluorination, giving δ 18O between 9.8‰ and 16.7‰ ( n = 110). Quartz overgrowths in thin sections from 10 rocks were analyzed by ion microprobe and average δ 18O = 29.3 ± 1.0‰ (1SD, n = 161). Given the similarity, on average, of δ 18O for all detrital quartz grains and for all quartz overgrowths, samples with higher δ 18O(WR) values can be shown to have more cement. The quartz cement in the 53 rocks, calculated by mass balance, varies from <1 to 21 vol.% cement, with one outlier at 33 vol.% cement. Eolian samples have an average of 11% cement compared to marine samples, which average 4% cement. Two models for quartz cementation have been investigated: high temperature (50-110 °C) formation from ore-forming brines related to Mississippi Valley Type (MVT) mineralization and formation as silcretes at low temperature (10-30 °C). The homogeneity of δ 18O for quartz overgrowths determined by ion microprobe rules out a systematic regional variation of temperature as predicted for MVT brines and there are no other known heating events in these sediments that were never buried to depths >1 km. The data in this study suggest that quartz overgrowths formed as silcretes in the St. Peter Sandstone from meteoric water with δ 18O values of -10‰ to -5‰ at 10-30 °C. This interpretation runs counter to conventional wisdom based on fibrous or opaline silica cements suggesting that the formation of syntaxial quartz overgrowths requires higher temperatures. While metastable silica cements commonly form at high degrees of silica oversaturation following rapid break-down reactions of materials such as of feldspars or glass, the weathering of a clean quartz arenite is slower facilitating chemical equilibrium and precipitation of crystallographically oriented overgrowths of α-quartz.

Histological changes induced by CO2 laser microprobe specially designed for root canal sterilization: in vivo study.

PubMed

Kesler, G; Koren, R; Kesler, A; Hay, N; Gal, R

1998-10-01

Until now, no suitable delivery fiber has existed for CO2 laser endodontic radiation in the apical region, where it is most difficult to eliminate the pulp tissue using conventional methods. To overcome this problem, we have designed a microprobe that reaches closer to the apex, distributing the energy density to a smaller area of the root canal and thus favorably increasing the thermal effects. A CO2 laser microprobe coupled onto a special hand piece was attached to the delivery fiber of a Sharplan 15-F CO2 laser. The study was conducted on 30 vital maxillary or mandibulary, central, lateral, or premolar teeth destined for extraction due to periodontal problems. Twenty were experimentally treated with pulsed CO2 laser delivered by this newly developed fiber after conventional root canal preparation. Temperature measured at three points on the root surface during laser treatment did not exceed 38 degrees C. Ten teeth represented the control group, in which only root canal preparation was performed in the conventional method. Histological examination of the laser-treated teeth showed coagulation necrosis and vacuolization of the remaining pulp tissue in the root canal periphery. Primary and secondary dentin appeared normal in all cases treated with 15-F CO2 laser. Gram stain and bacteriologic examination revealed complete sterilization. These results demonstrate the unique capabilities of this special microprobe in sterilization of the root canal, with no thermal damage to the surrounding tissue. The combination of classical root canal preparation with CO2 laser irradiation using this special microprobe before closing the canal can drastically change the quality of root canal fillings.

Trace Element Zoning and Incipient Metamictization in a Lunar Zircon: Application of Three Microprobe Techniques

NASA Technical Reports Server (NTRS)

Wopenka, Brigitte; Jollife, Bradley L.; Zinner, Ernst; Kremser, Daniel T.

1996-01-01

We have determined major (Si, Zr, Hf), minor (Al, Y, Fe, P), and trace element (Ca, Sc, Ti, Ba, REE, Th, U) concentrations and Raman spectra of a zoned, 200 microns zircon grain in lunar sample 14161,7069, a quartz monzodiorite breccia collected at the Apollo 14 site. Analyses were obtained on a thin section in situ with an ion microprobe, an electron microprobe, and a laser Raman microprobe. The zircon grain is optically zoned in birefringence, a reflection of variable (incomplete) metamictization resulting from zo- nation in U and Th concentrations. Variations in the concentrations of U and Th correlate strongly with those of other high-field-strength trace elements and with changes in Raman spectral parameters. Concentrations of U and Th range from 21 to 55 ppm and 6 to 31 ppm, respectively, and correlate with lower Raman peak intensities, wider Raman peaks, and shifted Si-O peak positions. Concentrations of heavy rare earth elements range over a factor of three to four and correlate with intensities of fluorescence peaks. Correlated variations in trace element concentrations reflect the original magmatic differentiation of the parental melt approx. 4 b.y. ago. Degradation of the zircon structure, as reflected by the observed Raman spectral parameters, has occurred in this sample over a range of alpha-decay event dose from approx. 5.2 x 10(exp 14) to 1.4 x 10(exp 15) decay events per milligram of zircon, as calculated from the U and Th concentrations. This dose is well below the approx. 10(exp 16) events per milligram cumulative dose that causes complete metamictization and indicates that laser Raman microprobe spectroscopy is an analytical technique that is very sensitive to the radiation-induced damage in zircon.

Improved spatial resolution for U-series dating of opal at Yucca Mountain, Nevada, USA, using ion-microprobe and microdigestion methods

USGS Publications Warehouse

Paces, J.B.; Neymark, L.A.; Wooden, J.L.; Persing, H.M.

2004-01-01

Two novel methods of in situ isotope analysis, ion microprobe and microdigestion, were used for 230Th/U and 234U/238U dating of finely laminated opal hemispheres formed in unsaturated felsic tuff at Yucca Mountain, Nevada, proposed site for a high-level radioactive waste repository. Both methods allow analysis of layers as many as several orders of magnitude thinner than standard methods using total hemisphere digestion that were reported previously. Average growth rates calculated from data at this improved spatial resolution verified that opal grew at extremely slow rates over the last million years. Growth rates of 0.58 and 0.69 mm/m.y. were obtained for the outer 305 and 740 ??m of two opal hemispheres analyzed by ion microprobe, and 0.68 mm/m.y. for the outer 22 ??m of one of these same hemispheres analyzed by sequential microdigestion. These Pleistocene growth rates are 2 to 10 times slower than those calculated for older secondary calcite and silica mineral coatings deposited over the last 5 to 10 m.y. dated by the U-Pb method and may reflect differences between Miocene and Pleistocene seepage flux. The microdigestion data also imply that opal growth rates may have varied over the last 40 k.y. These data are the first indication that growth rates and associated seepage in the proposed repository horizon may correlate with changes in late Pleistocene climate, involving faster growth during wetter, cooler climates (glacial maximum), slower growth during transition climates, and no growth during the most arid climate (modern). Data collected at this refined spatial scale may lead to a better understanding of the hydrologic variability expected within the thick unsaturated zone at Yucca Mountain over the time scale of interest for radioactive waste isolation. ?? 2004 Elsevier Ltd.

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.

Arizona porphyry copper/hydrothermal deposits II: Crystal structure of ajoite, (K + Na)3Cu20Al3Si29O76(OH)16⋅∼8H2O

PubMed Central

Pluth, Joseph J.; Smith, Joseph V.

2002-01-01

A crystal from the type locality Ajo, AZ, yielded just enough intensity from streaked diffractions using synchrotron x-rays at the Advanced Photon Source to solve the crystal structure with composition (K + Na)3Cu20Al3Si29O76(OH)16⋅∼8H2O; triclinic, P1̄, a = 13.634(5) Å, b = 13.687(7), c = 14.522(7), α = 110.83(1)°, β = 107.21(1), γ = 105.68(1); refined to a final R = 12.5%. Electron microprobe analysis yielded a similar chemical composition that is slightly different from the combined chemical and electron microprobe analyses in the literature. The ajoite structure can be described as a zeolitic octahedral-tetrahedral framework that combines the alternate stacking of edge-sharing octahedral CuO6 layers and curved aluminosilicate layers and strings. Channels bounded by elliptical 12-rings and circular 8-rings of tetrahedra contain (K and Na) ions and water. The Al atoms occupy some of the Si tetrahedral sites. Each Cu atom has near-planar bonds to four oxygen atoms plus two longer distances that generate a distorted octahedron. Valence bond estimates indicate that 8 oxygen atoms of 46 are hydroxyl. Only one alkali atom was located in distorted octahedral coordination, and electron microprobe analyses indicate K and Na as major substituents. The water from chemical analysis presumably occurs as disordered molecules of zeolitic type not giving electron density from diffraction. The high R factor results from structural disorder and many weak intensities close to detection level. The crystal chemistry is compared with shattuckite, Cu5(SiO3)4(OH)2, and planchéite, Cu8Si8O22(OH)4⋅H2O, both found in oxidized copper deposits of Arizona but only the former directly with ajoite. PMID:12177404

Arizona porphyry copper/hydrothermal deposits II: crystal structure of ajoite, (K + Na)3Cu20Al3Si29O76(OH)16*~8H2O.

PubMed

Pluth, Joseph J; Smith, Joseph V

2002-08-20

A crystal from the type locality Ajo, AZ, yielded just enough intensity from streaked diffractions using synchrotron x-rays at the Advanced Photon Source to solve the crystal structure with composition (K + Na)3Cu20Al3Si29O76(OH)16* approximately 8H2O; triclinic, P1, a = 13.634(5) A, b = 13.687(7), c = 14.522(7), alpha = 110.83(1) degrees, beta = 107.21(1), gamma = 105.68(1); refined to a final R = 12.5%. Electron microprobe analysis yielded a similar chemical composition that is slightly different from the combined chemical and electron microprobe analyses in the literature. The ajoite structure can be described as a zeolitic octahedral-tetrahedral framework that combines the alternate stacking of edge-sharing octahedral CuO6 layers and curved aluminosilicate layers and strings. Channels bounded by elliptical 12-rings and circular 8-rings of tetrahedra contain (K and Na) ions and water. The Al atoms occupy some of the Si tetrahedral sites. Each Cu atom has near-planar bonds to four oxygen atoms plus two longer distances that generate a distorted octahedron. Valence bond estimates indicate that 8 oxygen atoms of 46 are hydroxyl. Only one alkali atom was located in distorted octahedral coordination, and electron microprobe analyses indicate K and Na as major substituents. The water from chemical analysis presumably occurs as disordered molecules of zeolitic type not giving electron density from diffraction. The high R factor results from structural disorder and many weak intensities close to detection level. The crystal chemistry is compared with shattuckite, Cu5(SiO3)4(OH)2, and planchéite, Cu8Si8O22(OH)4.H2O, both found in oxidized copper deposits of Arizona but only the former directly with ajoite.

Microprobe array with low impedance electrodes and highly flexible polyimide cables for acute neural recording.

PubMed

Kisban, S; Herwik, S; Seidl, K; Rubehn, B; Jezzini, A; Umiltà, M A; Fogassi, L; Stieglitz, T; Paul, O; Ruther, P

2007-01-01

This paper reports on a novel type of silicon-based microprobes with linear, two and three dimensional (3D) distribution of their recording sites. The microprobes comprise either single shafts, combs with multiple shafts or 3D arrays combining two combs with 9, 36 or 72 recording sites, respectively. The electrical interconnection of the probes is achieved through highly flexible polyimide ribbon cables attached using the MicroFlex Technology which allows a connection part of small lateral dimensions. For an improved handling, probes can be secured by a protecting canula. Low-impedance electrodes are achieved by the deposition of platinum black. First in vivo experiments proved the capability to record single action potentials in the motor cortex from electrodes close to the tip as well as body electrodes along the shaft.

Zinc in Entamoeba invadens.

NASA Technical Reports Server (NTRS)

Morgan, R. S.; Sattilaro, R. F.

1972-01-01

Atomic absorption spectroscopy, electron microprobe analysis, and dithizone staining of trophozoites and cysts of Entamoeba invadens demonstrate that these cells have a high concentration of zinc (approximately one picogram per cell or 1% of their dry weight). In the cysts of this organism, the zinc is confined to the chromatoid bodies, which previous work has shown to contain crystals of ribosomes. The chemical state and function of this zinc are unknown.

Petrology of 60035 - Evolution of a polymict ANT breccia

NASA Technical Reports Server (NTRS)

Warner, R. D.; Taylor, G. J.; Keil, K.

1980-01-01

Extensive analysis of the lunar rock sample 60035 with optical microscopy and electron microprobe methods show it to be a polymict ANT breccia partly coated with glass, containing abundant clasts which have troctolitic/noritic anorthosite compositions. At least two episodes of crushing and mixing were involved in the petrogenesis of 60035, and annealing and mineral equilibration have not been extensive since the formation of the breccia.

An overview of the facilities, activities, and developments at the University of North Texas Ion Beam Modification and Analysis Laboratory (IBMAL)

NASA Astrophysics Data System (ADS)

Rout, Bibhudutta; Dhoubhadel, Mangal S.; Poudel, Prakash R.; Kummari, Venkata C.; Pandey, Bimal; Deoli, Naresh T.; Lakshantha, Wickramaarachchige J.; Mulware, Stephen J.; Baxley, Jacob; Manuel, Jack E.; Pacheco, Jose L.; Szilasi, Szabolcs; Weathers, Duncan L.; Reinert, Tilo; Glass, Gary A.; Duggan, Jerry L.; McDaniel, Floyd D.

2013-07-01

The Ion Beam Modification and Analysis Laboratory (IBMAL) at the University of North Texas includes several accelerator facilities with capabilities of producing a variety of ion beams from tens of keV to several MeV in energy. The four accelerators are used for research, graduate and undergraduate education, and industrial applications. The NEC 3MV Pelletron tandem accelerator has three ion sources for negative ions: He Alphatross and two different SNICS-type sputter ion sources. Presently, the tandem accelerator has four high-energy beam transport lines and one low-energy beam transport line directly taken from the negative ion sources for different research experiments. For the low-energy beam line, the ion energy can be varied from ˜20 to 80 keV for ion implantation/modification of materials. The four post-acceleration beam lines include a heavy-ion nuclear microprobe; multi-purpose PIXE, RBS, ERD, NRA, and broad-beam single-event upset; high-energy ion implantation line; and trace-element accelerator mass spectrometry. The NEC 3MV single-ended Pelletron accelerator has an RF ion source mainly for hydrogen, helium and heavier inert gases. We recently installed a capacitive liner to the terminal potential stabilization system for high terminal voltage stability and high-resolution microprobe analysis. The accelerator serves a beam line for standard RBS and RBS/C. Another beamline for high energy focused ion beam application using a magnetic quadrupole lens system is currently under construction. This beam line will also serve for developmental work on an electrostatic lens system. The third accelerator is a 200 kV Cockcroft-Walton accelerator with an RF ion source. The fourth accelerator is a 2.5 MV Van de Graaff accelerator, which was in operation for last several decades is currently planned to be used mainly for educational purpose. Research projects that will be briefly discussed include materials synthesis/modification for photonic, electronic, and magnetic applications, surface sputtering and micro-fabrication of materials, development of high-energy ion microprobe systems, and educational and outreach activities.

An overview of the facilities, activities, and developments at the University of North Texas Ion Beam Modification and Analysis Laboratory (IBMAL)

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

Rout, Bibhudutta; Dhoubhadel, Mangal S.; Poudel, Prakash R.

2013-07-03

The Ion Beam Modification and Analysis Laboratory (IBMAL) at the University of North Texas includes several accelerator facilities with capabilities of producing a variety of ion beams from tens of keV to several MeV in energy. The four accelerators are used for research, graduate and undergraduate education, and industrial applications. The NEC 3MV Pelletron tandem accelerator has three ion sources for negative ions: He Alphatross and two different SNICS-type sputter ion sources. Presently, the tandem accelerator has four high-energy beam transport lines and one low-energy beam transport line directly taken from the negative ion sources for different research experiments. Formore » the low-energy beam line, the ion energy can be varied from {approx}20 to 80 keV for ion implantation/modification of materials. The four post-acceleration beam lines include a heavy-ion nuclear microprobe; multi-purpose PIXE, RBS, ERD, NRA, and broad-beam single-event upset; high-energy ion implantation line; and trace-element accelerator mass spectrometry. The NEC 3MV single-ended Pelletron accelerator has an RF ion source mainly for hydrogen, helium and heavier inert gases. We recently installed a capacitive liner to the terminal potential stabilization system for high terminal voltage stability and high-resolution microprobe analysis. The accelerator serves a beam line for standard RBS and RBS/C. Another beamline for high energy focused ion beam application using a magnetic quadrupole lens system is currently under construction. This beam line will also serve for developmental work on an electrostatic lens system. The third accelerator is a 200 kV Cockcroft-Walton accelerator with an RF ion source. The fourth accelerator is a 2.5 MV Van de Graaff accelerator, which was in operation for last several decades is currently planned to be used mainly for educational purpose. Research projects that will be briefly discussed include materials synthesis/modification for photonic, electronic, and magnetic applications, surface sputtering and micro-fabrication of materials, development of high-energy ion microprobe systems, and educational and outreach activities.« less

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.

DSMC Simulations of Blunt Body Flows for Mars Entries: Mars Pathfinder and Mars Microprobe Capsules

NASA Technical Reports Server (NTRS)

Moss, James N.; Wilmoth, Richard G.; Price, Joseph M.

1997-01-01

The hypersonic transitional flow aerodynamics of the Mars Pathfinder and Mars Microprobe capsules are simulated with the direct simulation Monte Carlo method. Calculations of axial, normal, and static pitching coefficients were obtained over an angle of attack range comparable to actual flight requirements. Comparisons are made with modified Newtonian and free-molecular-flow calculations. Aerothermal results were also obtained for zero incidence entry conditions.

Lateral diffusion study of the Pt-Al system using the NAC nuclear microprobe.

NASA Astrophysics Data System (ADS)

de Waal, H.; Pretorius, R.

1999-10-01

In this study a nuclear microprobe (NMP) was used to analyse phase formation during reaction in Pt-Al lateral diffusion couples. Phase identification was done by Rutherford backscattering spectroscopy. These results were compared with phase formation during conventional thin film Pt-Al interactions. The co-existence of multiple phases in lateral diffusion couples is discussed with reference to the effective heat of formation (EHF) model.

Electrophysiological and Electrochemical Methods Development for the Detection of Biologically Active Chemical Agents

DTIC Science & Technology

1988-11-01

Bilayer ........................................... 14 5. Current-Voltage Curve for Gramacidin in a Lecithin -Sphingomyelin Patch Bilayer... lecithin (Avanti). 9 2. MATERIALS 2.1 Patch Microprobe Instrumentation. The basis of the microprobe system is an AxoPatch Patch- Clamping Amplifier System...histogram of 1024 events cut above 2 pA. Events sampled are thought to be from the same single gramacidin channel in a lecithin : sphingomyelin (5:1) patch

Pure phase encode magnetic field gradient monitor.

PubMed

Han, Hui; MacGregor, Rodney P; Balcom, Bruce J

2009-12-01

Numerous methods have been developed to measure MRI gradient waveforms and k-space trajectories. The most promising new strategy appears to be magnetic field monitoring with RF microprobes. Multiple RF microprobes may record the magnetic field evolution associated with a wide variety of imaging pulse sequences. The method involves exciting one or more test samples and measuring the time evolution of magnetization through the FIDs. Two critical problems remain. The gradient waveform duration is limited by the sample T(2)*, while the k-space maxima are limited by gradient dephasing. The method presented is based on pure phase encode FIDs and solves the above two problems in addition to permitting high strength gradient measurement. A small doped water phantom (1-3 mm droplet, T(1), T(2), T(2)* < 100 micros) within a microprobe is excited by a series of closely spaced broadband RF pulses each followed by FID single point acquisition. Two trial gradient waveforms have been chosen to illustrate the technique, neither of which could be measured by the conventional RF microprobe measurement. The first is an extended duration gradient waveform while the other illustrates the new method's ability to measure gradient waveforms with large net area and/or high amplitude. The new method is a point monitor with simple implementation and low cost hardware requirements.

The Mars Microprobe Mission: Advanced Micro-Avionics for Exploration Surface

NASA Astrophysics Data System (ADS)

Blue, Randel

2000-01-01

The Mars Microprobe Mission is the second spacecraft developed as part of the New Millennium Program deep space missions. The objective of the Microprobe Project is to demonstrate the applicability of key technologies for future planetary missions by developing two probes for deployment on Mars. The probes are designed with a single stage entry, descent, and landing system and impact the Martian surface at speeds of approximately 200 meters per second. The microprobes are composed of two main sections, a forebody section that penetrates to a depth below the Martian surface of 0.5 to 2 meters, and an aftbody section that remains on the surface. Each probe system consists of a number of advanced technology components developed specifically for this mission. These include a non-erosive aeroshell for entry into. the atmosphere, a set of low temperature batteries to supply probe power, an advanced microcontroller to execute the mission sequence, collect the science data, and react to possible system fault conditions, a telecommunications subsystem implemented on a set of custom integrated circuits, and instruments designed to provide science measurements from above and below the Martian surface. All of the electronic components have been designed and fabricated to withstand the severe impact shock environment and to operate correctly at predicted temperatures below -100 C.

Optical Fourier diffractometry applied to degraded bone structure recognition

NASA Astrophysics Data System (ADS)

Galas, Jacek; Godwod, Krzysztof; Szawdyn, Jacek; Sawicki, Andrzej

1993-09-01

Image processing and recognition methods are useful in many fields. This paper presents the hybrid optical and digital method applied to recognition of pathological changes in bones involved by metabolic bone diseases. The trabecular bone structure, registered by x ray on the photographic film, is analyzed in the new type of computer controlled diffractometer. The set of image parameters, extracted from diffractogram, is evaluated by statistical analysis. The synthetic image descriptors in discriminant space, constructed on the base of 3 training groups of images (control, osteoporosis, and osteomalacia groups) by discriminant analysis, allow us to recognize bone samples with degraded bone structure and to recognize the disease. About 89% of the images were classified correctly. This method after optimization process will be verified in medical investigations.

Correlation Between the Extent of Catalytic Activity and Charge Density of Montmorillonites

PubMed Central

Steudel, Annett; Emmerich, Katja; Lagaly, Gerhard; Schuhmann, Rainer

2010-01-01

Abstract The clay mineral montmorillonite is a member of the phyllosilicate group of minerals, which has been detected on martian soil. Montmorillonite catalyzes the condensation of activated monomers to form RNA-like oligomers. Extent of catalysis, that is, the yield of oligomers, and the length of the longest oligomer formed in these reactions widely varies with the source of montmorillonite (i.e., the locality where the mineral is mined). This study was undertaken to establish whether there exists a correlation between the extent of catalytic property and the charge density of montmorillonites. Charge density was determined by saturating the montmorillonites with alkyl ammonium cations that contained increasing lengths of alkyl chains, [CH3-(CH2)n-NH3]+, where n = 3–16 and 18, and then measuring d(001), interlayer spacing of the resulting montmorillonite-alkyl ammonium-montmorillonite complex by X-ray diffractometry (XRD). Results demonstrate that catalytic activity of montmorillonites with lower charge density is superior to that of higher charge density montmorillonite. They produce longer oligomers that contain 9 to 10 monomer units, while montmorillonite with high charge density catalyzes the formation of oligomers that contain only 4 monomer units. The charge density of montmorillonites can also be calculated from the chemical composition if elemental analysis data of the pure mineral are available. In the next mission to Mars, CheMin (Chemistry and Mineralogy), a combined X-ray diffraction/X-ray fluorescence instrument, will provide information on the mineralogical and elemental analysis of the samples. Possible significance of these results for planning the future missions to Mars for the search of organic compounds and extinct or extant life is discussed. Key Words: Mars—Origin of life—Montmorillonite—Mineral catalysis—Layer charge density—X–ray diffractometry. Astrobiology 10, 743–749. PMID:20854214

Light stable isotope analysis of meteorites by ion microprobe

NASA Technical Reports Server (NTRS)

Mcsween, Harry Y., Jr.

1994-01-01

The main goal was to develop the necessary secondary ion mass spectrometer (SIMS) techniques to use a Cameca ims-4f ion microprobe to measure light stable isotope ratios (H, C, O and S) in situ and in non-conducting mineral phases. The intended application of these techniques was the analysis of meteorite samples, although the techniques that have been developed are equally applicable to the investigation of terrestrial samples. The first year established techniques for the analysis of O isotope ratios (delta O-18 and delta O-17) in conducting mineral phases and the measurement of S isotope ratios (delta S-34) in a variety of sulphide phases. In addition, a technique was developed to measure delta S-34 values in sulphates, which are insulators. Other research undertaken in the first year resulted in SIMS techniques for the measurement of wide variety of trace elements in carbonate minerals, with the aim of understanding the nature of alteration fluids in carbonaceous chondrites. In the second year we developed techniques for analyzing O isotope ratios in nonconducting mineral phases. These methods are potentially applicable to the measurement of other light stable isotopes such as H, C and S in insulators. Also, we have further explored the analytical techniques used for the analysis of S isotopes in sulphides by analyzing troilite in a number of L and H ordinary chondrites. This was done to see if there was any systematic differences with petrological type.

A Two-Dimensional Multielectrode Microprobe for the Visual Cortex.

DTIC Science & Technology

1979-12-01

used in studies of the auditory nerve (Ref 5t494-500) and studies of cortical electrical activity during seizures (Ref 6s414). Since silicon is the...Master of Science by 7> Joseph A. Tatman 2Lt USAF Graduate Electrical Engineering December 1979 Approved for public releases distribution unlimited s...designed around this microprobe to detect- the cortico- electrical C , signas, multiplex and modulate these data, and then transmit them across the

The evolution of high-alumina basalts of the Klyuchevskoy volcano, Kamchatka, Russia, based on microprobe analyses of mineral inclusions

NASA Astrophysics Data System (ADS)

Ozerov, Alexei Y.

2000-01-01

The origin of calc-alkaline high-alumina basalts (HAB) of the Klyuchevskoy volcano, Kamchatka, was examined using electron microprobe analyses of phenocrysts and mineral phases included in the phenocrysts. Continuous trends on major-element variation diagrams suggest the HAB were derived from high-magnesia basalt (HMB) by fractional crystallization. Phenocrysts in the HAB are strongly zoned: olivine (Mg# 91-64), clinopyroxene (Wo 45-38En 40-51Fs 5-20) and chrome—spinel/magnetite inclusions in them (Cr 2O 3 45-0 wt.%, TiO 2 0.5-11%). Microprobe analyses of minerals included in the phenocrysts provide additional constraints on the mineral crystallization trends in the HAB. Fe/Mg partitioning data, when applied to the phenocrysts cores, show they crystallized from a HMB. The similarity of phenocryst core compositions in HAB with those in HMB strongly suggests a genetic relationship between the two magma types.

Sensing surface mechanical deformation using active probes driven by motor proteins

PubMed Central

Inoue, Daisuke; Nitta, Takahiro; Kabir, Arif Md. Rashedul; Sada, Kazuki; Gong, Jian Ping; Konagaya, Akihiko; Kakugo, Akira

2016-01-01

Studying mechanical deformation at the surface of soft materials has been challenging due to the difficulty in separating surface deformation from the bulk elasticity of the materials. Here, we introduce a new approach for studying the surface mechanical deformation of a soft material by utilizing a large number of self-propelled microprobes driven by motor proteins on the surface of the material. Information about the surface mechanical deformation of the soft material is obtained through changes in mobility of the microprobes wandering across the surface of the soft material. The active microprobes respond to mechanical deformation of the surface and readily change their velocity and direction depending on the extent and mode of surface deformation. This highly parallel and reliable method of sensing mechanical deformation at the surface of soft materials is expected to find applications that explore surface mechanics of soft materials and consequently would greatly benefit the surface science. PMID:27694937

Effect of chromium and phosphorus on the physical properties of iron and titanium-based amorphous metallic alloy films

NASA Technical Reports Server (NTRS)

Distefano, S.; Rameshan, R.; Fitzgerald, D. J.

1991-01-01

Amorphous iron and titanium-based alloys containing various amounts of chromium, phosphorus, and boron exhibit high corrosion resistance. Some physical properties of Fe and Ti-based metallic alloy films deposited on a glass substrate by a dc-magnetron sputtering technique are reported. The films were characterized using differential scanning calorimetry, stress analysis, SEM, XRD, SIMS, electron microprobe, and potentiodynamic polarization techniques.

In situ 40K-40Ca ‘double-plus’ SIMS dating resolves Klokken feldspar 40K-40Ar paradox

NASA Astrophysics Data System (ADS)

Harrison, T. Mark; Heizler, Matthew T.; McKeegan, Kevin D.; Schmitt, Axel K.

2010-11-01

The 40K- 40Ca decay system has not been widely utilized as a geochronometer because quantification of radiogenic daughter is difficult except in old, extremely high K/Ca domains. Even these environments have not heretofore been exploited by ion microprobe analysis due to the very high mass resolving power (MRP) of 25,000 required to separate 40K + from 40Ca +. We introduce a method that utilizes doubly-charged K and Ca species which permits isotopic measurements to be made at relatively low MRP (~ 5000). We used this K-Ca 'double-plus' approach to address an enduring controversy in 40Ar/ 39Ar thermochronology revolving around exsolved alkali feldspars from the 1166 Ma Klokken syenite (southern Greenland). Ion microprobe 40K- 40Ca analysis of Klokken samples reveal both isochron and pseudoisochron behaviors that reflect episodic isotopic and chemical exchange of coarsely exsolved perthites and a near end-member K-feldspar until ≤ 719 Ma, and perhaps as late at ~ 400 Ma. Feldspar microtextures in the Klokken syenite evolved over a protracted interval by non-thermal processes (fluid-assisted recrystallization) and thus this sample makes a poor model from which to address the general validity of 40Ar/ 39Ar thermochronological methodologies.

An external milli-beam for archaeometric applications on the AGLAE IBA facility of the Louvre museum

NASA Astrophysics Data System (ADS)

Calligaro, T.; Dran, J.-C.; Hamon, H.; Moignard, B.; Salomon, J.

1998-03-01

External beam lines have been built on numerous IBA facilities for the analysis of works of art to avoid sampling and vacuum potentially detrimental to the integrity of such precious objects. On the other hand, growing interest lies on microprobe systems which provide a high lateral resolution but which usually work under vacuum. Until recently, the AGLAE facility was equipped with separate external beam and microprobe lines. The need of a better spatial resolution in the external beam mode has led us to combine them into a single system which exhibits numerous advantages and allows the analysis of small heterogeneities like inclusions in gemstones or tiny components of composite samples. The triplet of quadrupole lenses bought from Oxford is used to focus the beam. By using a 0.75 μm thick Al foil as the exit window, blowing a helium flow around the beam spot and reducing the window-sample distance below 3 mm, a beam size of about 30 μm can be reached. The experimental setup includes two Si(Li), a HPGe and a Si surface barrier detectors for the simultaneous implementation of PIXE, NRA and RBS. The full description of this device is given as well as a few applications to highlight its capability.

A clinical pathologic study of mercurialentis medicamentosus.

PubMed

Garron, L K; Wood, I S; Spencer, W H; Hayes, T L

1976-01-01

Thirty-one patients who used eye drops containing the preservative, phenylmercuric nitrate for from 3 to 15 years, developed a brownish pigmentation of the anterior capsule of the pupillary area. Light and electron microscopic studies on two lenses demonstrated deposits of dense particulate material resembling melanin pigment on and in the anterior capsule of the lens in the area of the pupil. Special studies, including electron microprobe analysis and neutron activation analysis established the presence of mercury in a lens with mercurialentis. No mercury was found in two lenses used as controls.

Effect of thermal history on Mossbauer signature and hyperfine interaction parameters of copper ferrite

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

Modi, K. B., E-mail: kunalbmodi2003@yahoo.com; Raval, P. Y.; Dulera, S. V.

Two specimens of copper ferrite, CuFe{sub 2}O{sub 4}, have been synthesized by double sintering ceramic technique with different thermal history i.e. slow cooled and quenched. X-ray diffractometry has confirmed single phase fcc spinel structure for slow cooled sample while tetragonal distortion is present in quenched sample. Mossbauer spectral analysis for slow-cooled copper ferrite reveals super position of two Zeeman split sextets along with paramagnetic singlet in the centre position corresponds to delafossite (CuFeO{sub 2}) phase that is completely absent in quenched sample. The hyperfine interaction parameters are highly influenced by heat treatment employed.

Preparation and analysis of multilayer composites based on polyelectrolyte complexes

NASA Astrophysics Data System (ADS)

Petrova, V. A.; Orekhov, A. S.; Chernyakov, D. D.; Baklagina, Yu. G.; Romanov, D. P.; Kononova, S. V.; Volod'ko, A. V.; Ermak, I. M.; Klechkovskaya, V. V.; Skorik, Yu. A.

2016-11-01

A method for preparing multilayer film composites based on chitosan has been developed by the example of polymer pairs: chitosan-hyaluronic acid, chitosan-alginic acid, and chitosan-carrageenan. The structure of the composite films is characterized by X-ray diffractometry and scanning electron microscopy. It is shown that the deposition of a solution of hyaluronic acid, alginic acid, or carrageenan on a chitosan gel film leads to the formation of a polyelectrolyte complex layer at the interface, which is accompanied by the ordering of chitosan chains in the surface region; the microstructure of this layer depends on the nature of contacting polymer pairs.

Heats of immersion of titania powders in primer solutions

NASA Technical Reports Server (NTRS)

Siriwardane, R.; Wightman, J. P.

1983-01-01

The oxide layer present on titanium alloys can play an important role in determining the strength and durability of adhesive bonds. Here, three titania powders in different crystalline phases, rutile-R1, anatase-A1, and anatase-A2, are characterized by several techniques. These include microelectrophoresis, X-ray diffractometry, surface area pore volume analysis, X-ray photoelectron spectroscopy, and measurements of the heats of immersion. Of the three powders, R1 has the highest heat of immersion in water, while the interaction between water and A1 powder is low. Experimental data also suggest a specific preferential interaction of polyphenylquinoxaline with anatase.

Integrated otpical monitoring of MEMS for closed-loop control

NASA Astrophysics Data System (ADS)

Dawson, Jeremy M.; Wang, Limin; McCormick, W. B.; Rittenhouse, S. A.; Famouri, Parviz F.; Hornak, Lawrence A.

2003-01-01

Robust control and failure assessment of MEMS employed in physically demanding, mission critical applications will allow for higher degrees of quality assurance in MEMS operation. Device fault detection and closed-loop control require detailed knowledge of the operational states of MEMS over the lifetime of the device, obtained by a means decoupled from the system. Preliminary through-wafer optical monitoring research efforts have shown that through-wafer optical probing is suitable for characterizing and monitoring the behavior of MEMS, and can be implemented in an integrated optical monitoring package for continuous in-situ device monitoring. This presentation will discuss research undertaken to establish integrated optical device metrology for closed-loop control of a MUMPS fabricated lateral harmonic oscillator. Successful linear closed-loop control results using a through-wafer optical microprobe position feedback signal will be presented. A theoretical optical output field intensity study of grating structures, fabricated on the shuttle of the resonator, was performed to improve the position resolution of the optical microprobe position signal. Through-wafer microprobe signals providing a positional resolution of 2 μm using grating structures will be shown, along with initial binary Fresnel diffractive optical microelement design layout, process development, and testing results. Progress in the design, fabrication, and test of integrated optical elements for multiple microprobe signal delivery and recovery will be discussed, as well as simulation of device system model parameter changes for failure assessment.

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

Pratapa, S.; Susanti, L.; Insany, Y. A. S.

Simple coprecipitation method has been used to produce nanoparticles of MgO (magnesia), MgO{center_dot}Al{sub 2}O{sub 3}(spinel), Y{sub 2}O{sub 3}(yttria) and Fe{sub 3}O{sub 4}(ferrite). The raw materials were, in respective, magnesium powder, magnesium and aluminium powders, ytrria powder, and natural sand. The coprecipitation included the use of suitable acid and base to dissolve the powders or sand and to produce precipitates, as well as the use of water to wash and purify the precipitates, and drying at relatively low temperatures, namely lower than 100 deg. C, followed by heating at 450 deg. C, 750 deg. C, 600 deg. C and 200 deg.more » C to produce magnesia, spinel, yttria and ferrite nanopowders, respectively. X-ray diffractometry was used to characterise the purity and nanocrystallinity of the final powders. It was found qualitatively that the powders were of high purity. Further line-broadening analysis using single-line and Rietveld-based softwares was performed to reveal the nanocrystallinity of the powders. Different line breadth values were found for the powders, indicating different crystallite sizes. It was also found that, particularly for spinel and yttria, the diffraction peaks exhibited 'longer' tails, indicating broader crystallite size distribution. The average crystallite size for the powders ranged from 3 to 70 nm. The results could then be used as 'fingerprints' for nanocrystallinity using x-ray diffractometry. The XRD crystallite sizes for yttria and ferrite nanocrystals are in fair agreement with their counterparts from electron microscopy observation.« less

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.

Nuclear micro-probe analysis of Arabidopsis thaliana leaves

NASA Astrophysics Data System (ADS)

Ager, F. J.; Ynsa, M. D.; Domínguez-Solís, J. R.; López-Martín, M. C.; Gotor, C.; Romero, L. C.

2003-09-01

Phytoremediation is a cost-effective plant-based approach for remediation of soils and waters which takes advantage of the remarkable ability of some plants to concentrate elements and compounds from the environment and to metabolize various molecules in their tissues, such as toxic heavy metals and organic pollutants. Nowadays, phytoremediation technology is becoming of paramount importance when environmental decontamination is concerned, due to the emerging knowledge of its physiological and molecular mechanisms and the new biological and engineering strategies designed to optimize and improve it. In addition, the feasibility of using plants for environmental cleanup has been confirmed by many different trials around the world. Arabidopsis thaliana plants can be used for basic studies to improve the technology on phytoremediation. Making use of nuclear microscopy techniques, in this paper we study leaves of wild type and transgenic A. thaliana plants grown in a cadmium-rich environment under different conditions. Micro-PIXE, RBS and SEM analyses, performed on the scanning proton micro-probe at the CNA in Seville (Spain), prove that cadmium is preferentially sequestered in the central region of epidermal trichome and allow comparing the effects of genetic modifications.

Channeling STIM analysis of radiation damage in single crystal diamond membrane

NASA Astrophysics Data System (ADS)

Sudić, I.; Cosic, D.; Ditalia Tchernij, S.; Olivero, P.; Pomorski, M.; Skukan, N.; Jakšić, M.

2017-08-01

The use of focused ion beam transmission channeling patterns to monitor the damage creation process in thin diamond single crystal membrane is described. A 0.8 MeV proton beam from the Ruđer Bošković Institute nuclear microprobe was used to perform Channeling Scanning Transmission Ion Microscopy (CSTIM) measurements. CSTIM was used instead of RBS channeling because of (several orders of magnitude) lower damage done to the sample during the measurements. Damage was introduced in selected areas by 15 MeV carbon beam in range of fluences 3·1015-2·1017 ions/cm2. Contrary to Ion Beam Induced Charge (IBIC), CSTIM is shown to be sensitive to the large fluences of ion beam radiation. Complementary studies of both IBIC and CSTIM are presented to show that very high fluence range can be covered by these two microprobe techniques, providing much wider information about the diamond radiation hardness. In addition micro Raman measurements were performed and the height of the GR 1 peak was correlated to the ion beam fluence.

U, Th, Pb and REE abundances and Pb 207/Pb 206 ages of individual minerals in returned lunar material by ion microprobe mass analysis.

NASA Technical Reports Server (NTRS)

Andersen, C. A.; Hinthorne, J. R.

1972-01-01

Results of ion microprobe analyses of Apollo 11, 12 and 14 material, showing that U, Th, Pb and REE are concentrated in accessory minerals such as apatite, whitlockite, zircon, baddeleyite, zirkelite, and tranquillityite. Th/U ratios are found to vary by over a factor of 40 in these minerals. K, Ba, Rb and Sr have been localized in a K rich, U and Th poor glass phase that is commonly associated with the U and Th bearing accessory minerals. Li is observed to be fairly evenly distributed between the various accessory phases. The phosphates have been found to have REE abundance patterns (normalized to the chondrite abundances) that are fairly flat, while the Zr bearing minerals have patterns that rise steeply, by factors of ten or more, from La to Gd. All the accessory minerals have large negative Eu anomalies. Radiometric age dates (Pb 207/Pb 206) of the individual U and Th bearing minerals compare favorably with the Pb 207/Pb 206 age of the bulk rocks.

Phase transformations in 40-60-GPa shocked gneisses from the Haughton Crater (Canada): An Analytical Transmission Electron Microscopy (ATEM) study

NASA Technical Reports Server (NTRS)

Martinez, I.; Guyot, F.; Schaerer, U.

1992-01-01

In order to better understand phase transformations, chemical migration, and isotopic disequilibrium in highly shocked rocks, we have performed a microprobe and an ATEM study on gneisses shocked up to 60 GPa from the Haughton Crater. This study reveals the following chemical and structural characteristics: (1) SiO2 dominant areas are formed by a mixture of pure SiO2 polycrystalline quartz identified by electron diffraction pattern and chemical analysis and a silica-rich amorphous phase containing minor amounts of aluminium, potassium, and iron; (2) Areas with biotitelike composition are formed by less than 200-nm grains of iron-rich spinels embedded in a silica-rich amorphous phase that is very similar to the one described above; (3) Layers with feldsparlike composition are constituted by 100-200-nm-sized alumina-rich grains (the indexation of the crystalline structure is under progress) and the silica-rich amorphous phase; (4) Zones characterized by the unusual Al/Si ratio close to 1 are formed by spinel grains (200-nm-sized) embedded in the same silica-rich amorphous phase; and (5) The fracturated sillimanites contain domains with a lamellar structure, defined by the intercalation of 100-nm-wide lamellae of mullite crystals and of a silica-rich amorphous phase. These mullite crystals preserved the crystallographical orientation of the preshock sillimanite. All compositional domains, identified at the microprobe scale, can thus be explained by a mixture in different proportion between the following phases: (1) a silica-rich amorphous phase, with minor Al and K; (2) quartz crystals; (3) spinel crystals and alumina-rich crystals; (4) sillimanite; and (5) mullite. Such mixtures of amorphous phases and crystals in different proportions explain disturbed isotope systems in these rocks and chemical heterogeneities observed on the microprobe.

CL-imaging and ion microprobe dating of single zircons from a high-grade rock from the Central Zone, Limpopo Belt, South Africa: Evidence for a single metamorphic event at ˜2.0 Ga

NASA Astrophysics Data System (ADS)

Mouri, H.; Brandl, G.; Whitehouse, M.; de Waal, S.; Guiraud, M.

2008-02-01

The combination of ion microprobe dating and cathodoluminescence (CL) imaging of zircons from a high-grade rock from the Central Zone of the Limpopo Belt were used to constrain the age of metamorphic events in the area. Zircon grains extracted from an orthopyroxene-gedrite-bearing granulite were prepared for single crystal CL-imaging and ion microprobe dating. The grains display complex zoning when using SEM-based CL-imaging. A common feature in most grains is the presence of a distinct core with a broken oscillatory zoned structure, which clearly appears to be the remnant of an original grain of igneous origin. This core is overgrown by an unzoned thin rim measuring about 10-30 μm in diameter, which is considered as new zircon growth during a single metamorphic event. Selected domains of the zircon grains were analysed for U, Pb and Th isotopic composition using a CAMECA IMS 1270 ion microprobe (Nordsim facility). Most of the grains define a near-concordant cluster with some evidence of Pb loss. The most concordant ages of the cores yielded a weighted mean 207Pb/ 206Pb age of 2689 ± 15 (2 σ) Ma, interpreted as the age of the protolith of an igneous origin. The unzoned overgrowths of the zircon grains yielded a considerably younger weighted mean 207Pb/ 206Pb age of ˜2006.5 ± 8.0 Ma (2 σ), and these data are interpreted to reflect closely the age of the ubiquitous high-grade metamorphic event in the Central Zone. This study shows clearly, based on both the internal structure of the zircons and the data obtained by ion microprobe dating, that only a single metamorphic event is recorded by the studied 2.69 Ga old rocks, and we found no evidence of an earlier metamorphic event at ˜2.5 Ga as postulated earlier by some workers.

Boron Carbide Aluminum Cermets for External Pressure Housing Applications

DTIC Science & Technology

1992-09-01

CHEMISTRY AND MICROSTRUCTURES OF THE B4C/Al SYSTEM ......................................... 4 3.2 MECHANICAL PROPERTIES OF B4C/AI COMPOSITES ....... 10...TABLES 1. Phase chemistry of B4C/A1 composites as a function of baking temperature (by stereology) .................. ...... 10 2. Summary of the...diffractometer using CuKo radiation and a scan rate of 2° per minute. The chemistry of all phases was determined from electron microprobe analysis of

Ilmenite exsolution schemes in Apollo-17 high-Ti basalts

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

Vaniman, D.; Heiken, G.; Muhich, T.

1990-01-01

Combined electron microprobe and scanning electron microscope (SEM) x-ray image analyses are used to obtain semiquantitative data on the relations between ilmenite grains and their exsolved chromite and rutile. Comparisons of these data for ilmenites in four Apollo-17 high-Ti basalts with a database of electron microprobe analyses from the literature indicates that Cr expulsion from ilmenite can be as important as Fe{sup 2+} reduction in causing subsolidus exsolution of chromite and rutile from ilmenite. 12 refs., 4 figs., 5 tabs.

Use of electron microprobe x-ray analysis for determination of low calcium concentrations across leaves deficient in calcium

NASA Technical Reports Server (NTRS)

Barta, D. J.; Tibbitts, T. W.

1991-01-01

An electron microprobe with wavelength-dispersive x-ray spectrometry (WDS) was found to be useful for the determination of Ca concentrations in leaf tissue deficient in Ca. WDS effectively detected Ca concentrations as low as 0.2 mg/g dry wt in the presence of high levels of K and Mg (120 and 50 mg/g dry wt, respectively). Leaf specimens were prepared for analysis by quick-freezing in liquid nitrogen and freeze-drying at -20 degrees C to maintain elemental integrity within the tissue. Because dry material was analyzed, sample preparation was simple and samples could be stored for long periods before analysis. A large beam diameter of 50 gm was used to minimize tissue damage under the beam and analyze mineral concentrations within several cells at one time. Beam penetration was between 50 and 55 microns, approximately one-third of the thickness of the leaf. For analysis of concentrations in interveinal areas, analyses directed into the abaxial epidermis were found most useful. However, because of limited beam penetration, analyses of veinal areas would require use of cross sections [correction of crosssections]. Solid mineral standards were used for instrument standardization. To prevent measurement errors resulting from differences between the matrix of the mineral standards and the analyzed tissue, concentrations in leaves were corrected using gelatin standards prepared and analyzed under the same conditions. WDS was found to be useful for documenting that very low Ca levels occur in specific areas of lettuce leaves exhibiting the Ca deficiency injury termed tipburn.

KSC-98pc1645

NASA Image and Video Library

1998-11-12

KENNEDY SPACE CENTER, FLA. -- In the Spacecraft Assembly and Encapsulation Facility -2 (SAEF-2), JPL workers mount a Mars microprobe onto the Mars Polar Lander. Two microprobes will hitchhike on the lander, scheduled to be launched Jan. 3, 1999, aboard a Delta II rocket. The solar-powered spacecraft is designed to touch down on the Martian surface near the northern-most boundary of the south pole in order to study the water cycle there. The lander also will help scientists learn more about climate change and current resources on Mars, studying such things as frost, dust, water vapor and condensates in the Martian atmosphere. The Mars microprobes, called Deep Space 2, are part of NASA's New Millennium Program. They will complement the climate-related scientific focus of the lander by demonstrating an advanced, rugged microlaser system for detecting subsurface water. Such data on polar subsurface water, in the form of ice, should help put limits on scientific projections for the global abundance of water on Mars

KSC-98pc1647

NASA Image and Video Library

1998-11-12

KENNEDY SPACE CENTER, FLA. -- In the Spacecraft Assembly and Encapsulation Facility -2 (SAEF-2), JPL workers prepare to mount a Mars microprobe onto the Mars Polar Lander. Two microprobes will hitchhike on the lander, scheduled to be launched Jan. 3, 1999, aboard a Delta II rocket. The solar-powered spacecraft is designed to touch down on the Martian surface near the northern-most boundary of the south pole in order to study the water cycle there. The lander also will help scientists learn more about climate change and current resources on Mars, studying such things as frost, dust, water vapor and condensates in the Martian atmosphere. The Mars microprobes, called Deep Space 2, are part of NASA's New Millennium Program. They will complement the climate-related scientific focus of the lander by demonstrating an advanced, rugged microlaser system for detecting subsurface water. Such data on polar subsurface water, in the form of ice, should help put limits on scientific projections for the global abundance of water on Mars

KSC-98pc1642

NASA Image and Video Library

1998-11-12

KENNEDY SPACE CENTER, FLA. -- In the Spacecraft Assembly and Encapsulation Facility -2 (SAEF-2), Chris Voorhees (front) watches while Satish Krishnan (back) places a Mars microprobe on a workstand. Two microprobes will hitchhike on the Mars Polar Lander, scheduled to be launched Jan. 3, 1999, aboard a Delta II rocket. The solar-powered spacecraft is designed to touch down on the Martian surface near the northern-most boundary of the south pole in order to study the water cycle there. The lander also will help scientists learn more about climate change and current resources on Mars, studying such things as frost, dust, water vapor and condensates in the Martian atmosphere. The Mars microprobes, called Deep Space 2, are part of NASA's New Millennium Program. They will complement the climate-related scientific focus of the lander by demonstrating an advanced, rugged microlaser system for detecting subsurface water. Such data on polar subsurface water, in the form of ice, should help put limits on scientific projections for the global abundance of water on Mars

KSC-98pc1628

NASA Image and Video Library

1998-11-10

KENNEDY SPACE CENTER, FLA. -- In the Spacecraft Assembly and Encapsulation Facility -2 (SAEF-2), Satish Krishnan (right) from the Jet Propulsion Laboratory places a Mars microprobe on a workstand. In the background, Chris Voorhees watches. Two microprobes will hitchhike on the Mars Polar Lander, scheduled to be launched Jan. 3, 1999, aboard a Delta II rocket. The solar-powered spacecraft is designed to touch down on the Martian surface near the northern-most boundary of the south pole in order to study the water cycle there. The lander also will help scientists learn more about climate change and current resources on Mars, studying such things as frost, dust, water vapor and condensates in the Martian atmosphere. The Mars microprobes, called Deep Space 2, are part of NASA's New Millennium Program. They will complement the climate-related scientific focus of the lander by demonstrating an advanced, rugged microlaser system for detecting subsurface water. Such data on polar subsurface water, in the form of ice, should help put limits on scientific projections for the global abundance of water on Mars

KSC-98pc1641

NASA Image and Video Library

1998-11-12

KENNEDY SPACE CENTER, FLA. -- In the Spacecraft Assembly and Encapsulation Facility -2 (SAEF-2), Chris Voorhees (left) and Satish Krishnan (right), from the Jet Propulsion Laboratory, remove the second Mars microprobe from a drum. Two microprobes will hitchhike on the Mars Polar Lander, scheduled to be launched Jan. 3, 1999, aboard a Delta II rocket. The solar-powered spacecraft is designed to touch down on the Martian surface near the northern-most boundary of the south pole in order to study the water cycle there. The lander also will help scientists learn more about climate change and current resources on Mars, studying such things as frost, dust, water vapor and condensates in the Martian atmosphere. The Mars microprobes, called Deep Space 2, are part of NASA's New Millennium Program. They will complement the climate-related scientific focus of the lander by demonstrating an advanced, rugged microlaser system for detecting subsurface water. Such data on polar subsurface water, in the form of ice, should help put limits on scientific projections for the global abundance of water on Mars

Asymmetric Distribution of Metals in the Xenopus Laevis Oocyte: a Synchrotron X-Ray Fluorescence Microprobe Study

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

Popescu, B.F.Gh.; Belak, Z.R.; Ignatyev, K.

2009-06-04

The asymmetric distribution of many components of the Xenopus oocyte, including RNA, proteins, and pigment, provides a framework for cellular specialization during development. During maturation, Xenopus oocytes also acquire metals needed for development, but apart from zinc, little is known about their distribution. Synchrotron X-ray fluorescence microprobe was used to map iron, copper, and zinc and the metalloid selenium in a whole oocyte. Iron, zinc, and copper were asymmetrically distributed in the cytoplasm, while selenium and copper were more abundant in the nucleus. A zone of high copper and zinc was seen in the animal pole cytoplasm. Iron was alsomore » concentrated in the animal pole but did not colocalize with zinc, copper, or pigment accumulations. This asymmetry of metal deposition may be important for normal development. Synchrotron X-ray fluorescence microprobe will be a useful tool to examine how metals accumulate and redistribute during fertilization and embryonic development.« less

Asymmetri Distribution of Metals in the Xenopus Laevis Oocyte: a Synchrotron X-Ray Fluorescence Microprobe Study

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

Popescu, B.F.G.; Belak, Z.R.; Ignatyev, K.

2009-04-29

The asymmetric distribution of many components of the Xenopus oocyte, including RNA, proteins, and pigment, provides a framework for cellular specialization during development. During maturation, Xenopus oocytes also acquire metals needed for development, but apart from zinc, little is known about their distribution. Synchrotron X-ray fluorescence microprobe was used to map iron, copper, and zinc and the metalloid selenium in a whole oocyte. Iron, zinc, and copper were asymmetrically distributed in the cytoplasm, while selenium and copper were more abundant in the nucleus. A zone of high copper and zinc was seen in the animal pole cytoplasm. Iron was alsomore » concentrated in the animal pole but did not colocalize with zinc, copper, or pigment accumulations. This asymmetry of metal deposition may be important for normal development. Synchrotron X-ray fluorescence microprobe will be a useful tool to examine how metals accumulate and redistribute during fertilization and embryonic development.« less

KSC-98pc1643

NASA Image and Video Library

1998-11-12

KENNEDY SPACE CENTER, FLA. -- In the Spacecraft Assembly and Encapsulation Facility -2 (SAEF-2), a JPL worker checks the Mars microprobe. Two microprobes will hitchhike on the Mars Polar Lander, scheduled to be launched Jan. 3, 1999, aboard a Delta II rocket. The solar-powered spacecraft is designed to touch down on the Martian surface near the northern-most boundary of the south pole in order to study the water cycle there. The lander also will help scientists learn more about climate change and current resources on Mars, studying such things as frost, dust, water vapor and condensates in the Martian atmosphere. The Mars microprobes, called Deep Space 2, are part of NASA's New Millennium Program. They will complement the climate-related scientific focus of the lander by demonstrating an advanced, rugged microlaser system for detecting subsurface water. Such data on polar subsurface water, in the form of ice, should help put limits on scientific projections for the global abundance of water on Mars

KSC-98pc1648

NASA Image and Video Library

1998-11-12

KENNEDY SPACE CENTER, FLA. -- In the Spacecraft Assembly and Encapsulation Facility -2 (SAEF-2), the two Mars microprobes are shown mounted on opposite sides of the Mars Polar Lander. The two microprobes and the lander are scheduled to be launched Jan. 3, 1999, aboard a Delta II rocket. The solar-powered spacecraft is designed to touch down on the Martian surface near the northern-most boundary of the south pole in order to study the water cycle there. The lander also will help scientists learn more about climate change and current resources on Mars, studying such things as frost, dust, water vapor and condensates in the Martian atmosphere. The Mars microprobes, called Deep Space 2, are part of NASA's New Millennium Program. They will complement the climate-related scientific focus of the lander by demonstrating an advanced, rugged microlaser system for detecting subsurface water. Such data on polar subsurface water, in the form of ice, should help put limits on scientific projections for the global abundance of water on Mars

KSC-98pc1644

NASA Image and Video Library

1998-11-12

KENNEDY SPACE CENTER, FLA. -- In the Spacecraft Assembly and Encapsulation Facility -2 (SAEF-2), two JPL workers measure a Mars microprobe. Two microprobes will hitchhike on the Mars Polar Lander, scheduled to be launched Jan. 3, 1999, aboard a Delta II rocket. The solar-powered spacecraft is designed to touch down on the Martian surface near the northern-most boundary of the south pole in order to study the water cycle there. The lander also will help scientists learn more about climate change and current resources on Mars, studying such things as frost, dust, water vapor and condensates in the Martian atmosphere. The Mars microprobes, called Deep Space 2, are part of NASA's New Millennium Program. They will complement the climate-related scientific focus of the lander by demonstrating an advanced, rugged microlaser system for detecting subsurface water. Such data on polar subsurface water, in the form of ice, should help put limits on scientific projections for the global abundance of water on Mars

KSC-98pc1646

NASA Image and Video Library

1998-11-12

KENNEDY SPACE CENTER, FLA. -- In the Spacecraft Assembly and Encapsulation Facility -2 (SAEF-2), a JPL worker carries a Mars microprobe to the Mars Polar Lander at left. Two microprobes will hitchhike on the lander, scheduled to be launched Jan. 3, 1999, aboard a Delta II rocket. The solar-powered spacecraft is designed to touch down on the Martian surface near the northern-most boundary of the south pole in order to study the water cycle there. The lander also will help scientists learn more about climate change and current resources on Mars, studying such things as frost, dust, water vapor and condensates in the Martian atmosphere. The Mars microprobes, called Deep Space 2, are part of NASA's New Millennium Program. They will complement the climate-related scientific focus of the lander by demonstrating an advanced, rugged microlaser system for detecting subsurface water. Such data on polar subsurface water, in the form of ice, should help put limits on scientific projections for the global abundance of water on Mars

Chromium in urban sediment particulates: an integrated micro-chemical and XANES study

NASA Astrophysics Data System (ADS)

Taylor, Kevin; Byrne, Patrick; Hudson-Edwards, Karen

2015-04-01

Chromium is generally common within the urban sediment cascade as a result of abundant industrial and transport-related sources. The risks that Cr-bearing particles pose to ecosystems and humans depend on the solid phase chemical speciation of Cr in the particles. In this study, we use bulk chemical digests, sequential chemical extraction analysis, electron microscopy, electron microprobe and microfocus XANES analysis to describe the solid-phase speciation of Cr in urban particulate matter from both aquatic sediment and road dust sediment (RDS) in Manchester, UK. Cr-bearing grains within RDS are predominantly iron oxide grains, commonly of goethite or haematite mineralogy, but Cr-bearing silicate glass grains are also present. Iron oxide glass grains most likely have sorbed Cr, and derive from the rusting of Cr-steel particles from vehicles. Electron microprobe analysis indicates concentrations of Cr up to 3200 μg/g in these grains, and XANES analysis indicates that Cr(III) is the dominant oxidation state, with some trace amounts of Cr(VI). Cr-bearing grains within aquatic sediments are dominated by alumino-silicate glass grains derived from industrial waste. These grains contain Cr-rich areas with up to 19% Cr2O3 and XANES analysis indicates that Cr is present as Cr(III). The dominance of Cr(III) in these urban particulate grains suggests limited bioavailability or toxicity. However, the presence within two markedly different grain types (iron oxides and silicate glasses) indicates that the long-term geochemical behaviour and environmental risk of RDS and the aquatic sediments studied are likely to be quite different. These findings highlight the importance of understanding sources of metal contaminants in urban environments and the geochemical processes that affect their transfer through the urban sediment cascade and the wider river basin.

Workshop on Cometary Dust in Astrophysics

NASA Technical Reports Server (NTRS)

2003-01-01

The paper include contribution of each Lunar and Planetary Institute. Contents include the following: Mass flux in the ancient Earth-Moon system and benign implications for the origin of life on Earth. In-situ analysis of complex organic matter in cometary dust by ion microprobe. Pristine presolar silicon carbide. Infrared spectra of melilite solid solution. Comet observations with SIRTF. Ice and carbon chemistry in comets. The nature in interstellar dust. Modeling the infrared emission from protoplanetary dust disks.

ONR (Office of Naval Research) Far East Scientific Information Bulletin. Volume 13, Number 4, October-December 1988

DTIC Science & Technology

1988-12-01

by light finger pressure; and surface shaded or rubbed by soft pencil, charcoal, or crayon. Anglers initiated this custom as a means of recording...related to the barium titanate or simple nects, and mixers. Some of these applica- perovskite unit cell (Figure 1). In this struc- tions can be...dispersive spectroscopy (EDS), Target-~ microprobe analysis, and x-ray diffraction R~orOC(XRD). MagnetsOptical microscopy with polarized light

A Review of Positive Ion Sensitivities for the SIMS Analysis of CMT

DTIC Science & Technology

1991-05-01

microprobe. Inter-laboratory exercises organised by NRL using standardised glasses and steels’ s showed considerable agreement usually within a factor...would be sufficient oxygen to convert all the remaining matrix atoms to oxides, TeO2 and CdO. Any general theory of the lonisation of sputtered particles...Eggert equation which works well for many other matrices, such as metals, glasses and ceramics. Despite decades of basic studies there is still no

Hot-phonon generation in THz quantum cascade lasers

NASA Astrophysics Data System (ADS)

Spagnolo, V.; Vitiello, M. S.; Scamarcio, G.; Williams, B. S.; Kumar, S.; Hu, Q.; Reno, J. L.

2007-12-01

Observation of non-equilibrium optical phonons population associated with electron transport in THz quantum cascade lasers is reported. The phonon occupation number was measured by using a combination of micro-probe photoluminescence and Stokes/Anti-Stokes Raman spectroscopy. Energy balance analysis allows us to estimate the phonon relaxation rate, that superlinearly increases with the electrical power in the range 1.5 W - 1.95 W, above laser threshold. This observation suggests the occurrence of stimulated emission of optical phonons.

In-situ determination of metallic variation and multi-association in single particles by combining synchrotron microprobe, sequential chemical extraction and multivariate statistical analysis.

PubMed

Zhu, Yu-Min; Zhang, Hua; Fan, Shi-Suo; Wang, Si-Jia; Xia, Yi; Shao, Li-Ming; He, Pin-Jing

2014-07-15

Due to the heterogeneity of metal distribution, it is challenging to identify the speciation, source and fate of metals in solid samples at micro scales. To overcome these challenges single particles of air pollution control residues were detected in situ by synchrotron microprobe after each step of chemical extraction and analyzed by multivariate statistical analysis. Results showed that Pb, Cu and Zn co-existed as acid soluble fractions during chemical extraction, regardless of their individual distribution as chlorides or oxides in the raw particles. Besides the forms of Fe2O3, MnO2 and FeCr2O4, Fe, Mn, Cr and Ni were closely associated with each other, mainly as reducible fractions. In addition, the two groups of metals had interrelations with the Si-containing insoluble matrix. The binding could not be directly detected by micro-X-ray diffraction (μ-XRD) and XRD, suggesting their partial existence as amorphous forms or in the solid solution. The combined method on single particles can effectively determine metallic multi-associations and various extraction behaviors that could not be identified by XRD, μ-XRD or X-ray absorption spectroscopy. The results are useful for further source identification and migration tracing of heavy metals. Copyright © 2014 Elsevier B.V. All rights reserved.

Chemical fingerprinting and source tracing of obsidian: the central Mediterranean trade in black gold.

PubMed

Tykot, Robert H

2002-08-01

Chemical fingerprinting using major or trace element composition is used to characterize the Mediterranean island sources of obsidian and can even differentiate as many as nine flows in the Monte Arci region of Sardinia. Analysis of significant numbers of obsidian artifacts from Neolithic sites in the central Mediterranean reveals specific patterns of source exploitation and suggests particular trade mechanisms and routes. The use of techniques such as X-ray fluorescence, the electron microprobe, neutron activation analysis, and laser ablation ICP mass spectrometry are emphasized in order to produce quantitative results while minimizing damage to valuable artifacts.

Optical and chemical analysis of iron in Luna 20 plagioclase.

NASA Technical Reports Server (NTRS)

Bell, P. M.; Mao, H. K.

1973-01-01

Review of analytical data on the iron content of Luna 20 anorthitic plagioclase, obtained by a highly sensitive technique for measuring polarized absorption related to crystal-field splittings and by automated electron microprobe analysis of oriented single crystals. The iron content is found to range from a few hundredths to a few tenths of a weight per cent from crystal to crystal. The optical and chemical properties of the iron appear to be caused by postcrystallization migration and exsolution. Postcrystallization effects may obscure evidence of the original oxidation state and iron concentration of these crystals.

The x ray microprobe determination of chromium oxidation state in olivine from lunar basalt and kimberlitic diamonds

NASA Technical Reports Server (NTRS)

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

1993-01-01

The synchrotron x-ray microprobe is being used to obtain oxidation state information on planetary materials with high spatial resolution. Initial results on chromium in olivine from various sources including laboratory experiments, lunar basalt, and kimberlitic diamonds are reported. The lunar olivine was dominated by Cr(2+) whereas the diamond inclusions had Cr(2+/Cr(3+) ratios up to about 0.3. The simpliest interpretation is that the terrestrial olivine crystallized in a more oxidizing environment than the lunar olivine.

Nuclear microprobe investigation of the effects of ionization and displacement damage in vertical, high voltage GaN diodes

DOE PAGES

Vizkelethy, G.; King, M. P.; Aktas, O.; ...

2016-12-02

Radiation responses of high-voltage, vertical gallium-nitride (GaN) diodes were investigated using Sandia National Laboratories’ nuclear microprobe. Effects of the ionization and the displacement damage were studied using various ion beams. We found that the devices show avalanche effect for heavy ions operated under bias well below the breakdown voltage. Here, the displacement damage experiments showed a surprising effect for moderate damage: the charge collection efficiency demonstrated an increase instead of a decrease for higher bias voltages.

Nuclear microprobe investigation of the effects of ionization and displacement damage in vertical, high voltage GaN diodes

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

Vizkelethy, G.; King, M. P.; Aktas, O.

Radiation responses of high-voltage, vertical gallium-nitride (GaN) diodes were investigated using Sandia National Laboratories’ nuclear microprobe. Effects of the ionization and the displacement damage were studied using various ion beams. We found that the devices show avalanche effect for heavy ions operated under bias well below the breakdown voltage. Here, the displacement damage experiments showed a surprising effect for moderate damage: the charge collection efficiency demonstrated an increase instead of a decrease for higher bias voltages.

Elemental mapping of biological samples using a scanning proton microprobe

NASA Astrophysics Data System (ADS)

Watt, F.; Grime, G. W.

1988-03-01

Elemental mapping using a scanning proton microprobe (SPM) can be a powerful technique for probing trace elements in biology, allowing complex interfaces to be studied in detail, identifying contamination and artefacts present in the specimen, and in certain circumstances obtaining indirect chemical information. Examples used to illustrate the advantages of the technique include the elemental mapping of growing pollen tubes, honey bee brain section, a mouse macrophage cell, human liver section exhibiting primary biliary cirrhosis, and the attack by a mildew fungus on a pea leaf.

Gold Nanoparticles: An Efficient Antimicrobial Agent against Enteric Bacterial Human Pathogen

PubMed Central

Shamaila, Shahzadi; Zafar, Noshin; Riaz, Saira; Sharif, Rehana; Nazir, Jawad; Naseem, Shahzad

2016-01-01

Enteric bacterial human pathogens, i.e., Escherichia coli, Staphylococcus aureus, Bacillus subtilis and Klebsiella pneumoniae, are the major cause of diarrheal infections in children and adults. Their structure badly affects the human immune system. It is important to explore new antibacterial agents instead of antibiotics for treatment. This project is an attempt to explain how gold nanoparticles affect these bacteria. We investigated the important role of the mean particle size, and the inhibition of a bacterium is dose-dependent. Ultra Violet (UV)-visible spectroscopy revealed the size of chemically synthesized gold nanoparticle as 6–40 nm. Atomic force microscopy (AFM) analysis confirmed the size and X-ray diffractometry (XRD) analysis determined the polycrystalline nature of gold nanoparticles. The present findings explained how gold nanoparticles lyse Gram-negative and Gram-positive bacteria. PMID:28335198

The Role of the Ion Microprobe in Solid-Earth Geochemistry

NASA Astrophysics Data System (ADS)

Hauri, E. H.

2002-12-01

Despite the early success of the electron microprobe in taking petrology to the micron scale, and the widespread use of mass spectrometers in geochemistry and geochronology, it was not until the mid-1970s that the ion microprobe came into its own as an in situ analytical tool in the Earth sciences. Despite this inauspicious beginning, secondary ion mass spectrometry (SIMS) was widely advertised as a technology that would eventually eclipse thermal ion mass spectrometry (TIMS) in isotope geology. However this was not to happen. While various technical issues in SIMS such as interferences and matrix effects became increasingly clear, an appreciation grew for the complimentary abilities of SIMS and TIMS that, even with the advent of ICP-MS, continues to this day. Today the ion microprobe is capable of abundance measurements in the parts-per-billion range across nearly the entire periodic table, and SIMS stable isotope data quality is now routinely crossing the 1 per mil threshold, all at the micron scale. Much of this success is due to the existence of multi-user community facilities for SIMS research, and the substantial efforts of interested scientists to understand the fundamentals of sputtered ion formation and their application to geochemistry. Recent discoveries of evidence for the existence of ancient crust and oceans, the emergence of life on Earth, the large-scale cycling of surficial materials into the deep Earth, and illumination of fundamental high-pressure phenomena have all been made possible by SIMS, and these (and many more) discoveries owe a debt to the vision of creating and supporting multi-user community facilities for SIMS. The ion microprobe remains an expensive instrument to purchase and maintain, yet it is also exceedingly diverse in application. Major improvements in SIMS, indeed in all mass spectrometry, are visible on the near horizon. Yet the geochemical community cannot depend on commercial manufacturers alone to design and build the next generation of instrumentation for geochemistry. Such will be the role of instrument-minded scientists asking questions that simply cannot be answered by extant means. And it will be multi-user facilities that will make such advancements available to the wider geochemical community.

FUN with PANURGE - High mass resolution ion microprobe measurements of Mg in Allende inclusions. [meteoritic composition isotope analysis

NASA Technical Reports Server (NTRS)

Huneke, J. C.; Armstrong, J. T.; Wassserburg, G. J.

1983-01-01

Isotopic ratios have been determined, at a precision level approaching that of counting statistics using beam switching, by employing PANURGE, a modified CAMECA IMS3F ion microprobe at a mass resolving power of 5000. This technique is used to determine the isotopic composition of Mg and Si and the atomic ratio of Al/Mg in minerals from the Allende inclusion WA and the Allende FUN inclusion C1. Results show enrichment in Mg-26 of up to 260 percent. Results of Mg and Al/Mg measurements on cogenetic spinel inclusion and host plagiclase crystals show Mg-Al isochrons in excellent agreement with precise mineral isochrons determined by thermal emission mass spectrometry. The measurements are found to confirm the presence of substantial excess Mg-26 in WA and its near absence in C1. Data is obtained which indicates a metamorphic reequilibrium of Mg in Allende plagioclase at least 0.6 my after WA formation. Ion probe measurements are obtained which confirm that the Mg composition in Allende C1 is highly fractionated and is uniform among pyroxene, melilite, plagioclase, spinel crystals, and spinel included in melilite and plagioclase crystals.

Void formation in INCONEL MA-754 by high temperature oxidation

NASA Astrophysics Data System (ADS)

Rosenstein, Alan H.; Tien, John K.; Nix, William D.

1986-01-01

Subsurface void formation in oxide dispersion strengthened MA-754 caused by high temperature oxidation was investigated at temperatures of 1100, 1150, and 1200 °C for times of 1, 10, 50, and 100 hours. Material exposed at 1200 °C was examined using microprobe, SEM, and optical microscopy techniques. After exposure in air at 1200 °C for 100 hours, chromium depletion by as much as 10 wt pct was observed near the surface, and voids of various sizes up to 15 µm in diameter were found to depths of 300 µm. The fraction of voids increases with exposure time and, with the exception of anomalous values near the surface, decreases with depth. The maximum area fraction of voids observed was approximately 8 pct. Correlation of the void area fraction profile with the measured chromium depletion through a diffusion analysis shows that void formation is due to vacancy injection. Similar void formation in Ni-Cr alloys without oxide dispersions suggests that void formation is not dependent upon the presence of oxide dispersions. The diffusion coefficient for chromium in MA-754 at 1200 °C was computed from microprobe data to be 4 × 10-10 cm2 per second.

Force-displacement measurements of earlywood bordered pits using a mesomechanical tester.

PubMed

Zelinka, Samuel L; Bourne, Keith J; Hermanson, John C; Glass, Samuel V; Costa, Adriana; Wiedenhoeft, Alex C

2015-10-01

The elastic properties of pit membranes are reported to have important implications in understanding air-seeding phenomena in gymnosperms, and pit aspiration plays a large role in wood technological applications such as wood drying and preservative treatment. Here we present force-displacement measurements for pit membranes of circular bordered pits, collected on a mesomechanical testing system. The system consists of a quartz microprobe attached to a microforce sensor that is positioned and advanced with a micromanipulator mounted on an inverted microscope. Membrane displacement is measured from digital image analysis. Unaspirated pits from earlywood of never-dried wood of Larix and Pinus and aspirated pits from earlywood of dried wood of Larix were tested to generate force-displacement curves up to the point of membrane failure. Two failure modes were observed: rupture or tearing of the pit membrane by the microprobe tip, and the stretching of the pit membrane until the torus was forced out of the pit chamber through the pit aperture without rupture, a condition we refer to as torus prolapse. Published 2015. This article is a U.S. Government work and is in the public domain in the USA.

Development of a High Resolution-High Sensitivity Ion Microprobe Facility for Cosmochemical Applications

NASA Technical Reports Server (NTRS)

McKeegan, Kevin D.

1998-01-01

NASA NAGW-4112 has supported development of the CAMECA ims 1270 ion microprobe at UCLA for applications in cosmochemistry. The instrument has been brought to an operational status and techniques developed for accurate, precise microbeam analysis of oxygen isotope ratios in polished thin-sections. We made the first oxygen isotopic (delta(18)O and delta(17)O) measurements of rare mafic silicates in the most chemically primitive meteorites, the a chondrites (Leshin et al., 1997). The results have implications for both high temperature processing in the nebula and low-T aqueous alteration on the CI asteroid. We have performed measurements of oxygen isotopic compositions of magnetite and co-existing olivine from carbonaceous (Choi et al., 1997) and unequilibrated ordinary chondrites (Choi et al., in press). This work has identified a significant new oxygen isotope reservoir in the early solar system: water characterized by a very high Delta(17)) value of approx. 5 % per thousand. We have determined the spatial distributions of oxygen isotopic anomalies in all major mineral phases of a type B CAI from Allende. We have also studied an unusual fractionated CAI from Leoville and made the first oxygen isotopic measurements in rare CAIs from ordinary chondrites.

Background of SAM atom-fraction profiles

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

Ernst, Frank

Atom-fraction profiles acquired by SAM (scanning Auger microprobe) have important applications, e.g. in the context of alloy surface engineering by infusion of carbon or nitrogen through the alloy surface. However, such profiles often exhibit an artifact in form of a background with a level that anti-correlates with the local atom fraction. This article presents a theory explaining this phenomenon as a consequence of the way in which random noise in the spectrum propagates into the discretized differentiated spectrum that is used for quantification. The resulting model of “energy channel statistics” leads to a useful semi-quantitative background reduction procedure, which ismore » validated by applying it to simulated data. Subsequently, the procedure is applied to an example of experimental SAM data. The analysis leads to conclusions regarding optimum experimental acquisition conditions. The proposed method of background reduction is based on general principles and should be useful for a broad variety of applications. - Highlights: • Atom-fraction–depth profiles of carbon measured by scanning Auger microprobe • Strong background, varies with local carbon concentration. • Needs correction e.g. for quantitative comparison with simulations • Quantitative theory explains background. • Provides background removal strategy and practical advice for acquisition.« less

Analysis of microstructure and mechanical properties of aluminium-copper joints welded by FSW process

NASA Astrophysics Data System (ADS)

Iordache, M.; Sicoe, G.; Iacomi, D.; Niţu, E.; Ducu, C.

2017-08-01

The research conducted in this article aimed to check the quality of joining some dissimilar materials Al-Cu by determining the mechanical properties and microstructure analysis. For the experimental measurements there were used tin alloy Al - EN-AW-1050A with a thickness of 2 mm and Cu99 sheet with a thickness of 2 mm, joined by FSW weld overlay. The main welding parameters were: rotating speed of the rotating element 1400 rev/min, speed of the rotating element 50 mm/min. The experimental results were determined on samples specially prepared for metallographic analysis. In order to prepare samples for their characterization, there was designed and built a device that allowed simultaneous positioning and fixing for grinding. The characteristics analyzed in the joint welded samples were mictrostructure, microhardness and residual stresses. The techniques used to determine these characteristics were optical microscopy, electron microscopy with fluorescence radioactive elemental analysis (EDS), Vickers microhardness line - HV0.3 and X-ray diffractometry.

The Structure and Properties of Diffusion Assisted Bonded Joints in 17-4 PH, Type 347, 15-5 PH and Nitronic 40 Stainless Steels

NASA Technical Reports Server (NTRS)

Wigley, D. A.

1981-01-01

Diffusion assisted bonds are formed in 17-4 PH, 15-5 PH, type 347 and Nitronic 40 stainless steels using electrodeposited copper as the bonding agent. The bonds are analyzed by conventional metallographic, electron microprobe analysis, and scanning electron microscopic techniques as well as Charpy V-notch impact tests at temperatures of 77 and 300 K. Results are discussed in terms of a postulated model for the bonding process.

Dual fiber microprobe for mapping elemental distributions in biological cells

DOEpatents

Martin, Rodger C [Powell, TN; Martin, Madhavi Z [Powell, TN

2007-07-31

Laser-induced breakdown spectroscopy (LIBS) is applied on a microscale for in situ elemental analysis and spatial mapping in biological cells. A high power laser beam is focused onto a cell surface using a dual branching optical fiber probe for optical excitation of the cell constituents. Dual spectrometers and ICCD detectors capture the emission spectra from the excited cell(s). Repeated probing or repositioning of the laser beam with respect to the cell can provide 2-D or 3-D mapping of the cell.

KSC-98pc1629

NASA Image and Video Library

1998-11-10

KENNEDY SPACE CENTER, FLA. -- In the Spacecraft Assembly and Encapsulation Facility-2 (SAEF-2), Tandy Bianco, with Lockheed Martin, and Satish Krishnan (foreground) and Chris Voorhees (behind him), from the Jet Propulsion Laboratory, observe a Mars microprobe on the workstand. Two microprobes will hitchhike on the Mars Polar Lander, scheduled to be launched Jan. 3, 1999, aboard a Delta II rocket. The solar-powered spacecraft is designed to touch down on the Martian surface near the northern-most boundary of the south pole in order to study the water cycle there. The lander also will help scientists learn more about climate change and current resources on Mars, studying such things as frost, dust, water vapor and condensates in the Martian atmosphere. The Mars microprobes, called Deep Space 2, are part of NASA's New Millelnnium Program. They will complement the climate-related scientific focus of the lander by demonstrating an advanced, rugged microlaser system for detecting subsurface water. Such data on polar subsurface water, in the form of ice, should help put limits on scientific projections for the global abundance of water on Mars

Late Pleistocene granodiorite beneath Crater Lake caldera, Oregon, dated by ion microprobe

USGS Publications Warehouse

Bacon, C.R.; Persing, H.M.; Wooden, J.L.; Ireland, T.R.

2000-01-01

Variably melted granodiorite blocks ejected during the Holocene caldera-forming eruption of Mount Mazama were plucked from the walls of the climactic magma chamber ~15 km depth. Ion-microprobe U-Pb dating of zircons from two unmelted granodiorite blocks with SHRIMP RG (sensitive high-resolution ion microprobe-reverse geometry) gives a nominal 238U/206Pb age of 101+78-80 ka, or 174+89-115 ka when adjusted for an initial 230Th deficit. SHRIMP RG U-Th measurements on a subset of the zircons yield a 230Th/238U isochron age of 112 ?? 24 ka, considered to be the best estimate of the time of solidification of the pluton. These results suggest that the granodiorite is related to andesite and dacite of Mount Mazama and not to magmas of the climactic eruption. The unexposed granodiorite has an area of at least 28 km2. This young, shallow pluton was emplaced in virtually the same location where a similarly large magma body accumulated and powered violent explosive eruptions ~7700 yr ago, resulting in collapse of Crater Lake caldera.

Microsurgical laser Doppler probe for simultaneous intraoperative monitoring of cochlear blood flow and electrocochleography from the round window

NASA Astrophysics Data System (ADS)

Abiy, Lidet; Telischi, Fred; Parel, Jean-Marie A.; Manns, Fabrice; Saettele, Ralph; Morawski, Krzysztof; Ozdamar, Ozcan; Borgos, John; Delgado, Rafael; Miskiel, Edward; Yavuz, Erdem

2003-06-01

The aim of this project is the development of a microsurgical laser Doppler (LD) probe that simultaneously monitors blood flow and Electrocochleography (ECochG) from the round window of the ear. The device will prevent neurosensory hearing loss during acoustic neuroma surgery by preventing damage to the internal auditory nerve and to the cochlear blood flow supply. A commercially available 0.5 mm diameter Laser-Doppler velocimetry probe (LaserFlo, Vasamedics) was modified to integrate an ECochG electrode. A tube for suction and irrigation was incorporated into a sheath of the probe shaft, to facilitate cleaning of the round window (RW) and allow drug delivery to the round window membrane. The prototype microprobe was calibrated on a single vessel model and tested in vivo in a rabbit model. Preliminary results indicate that the microprobe was able to measure changes in cochlear blood flow (CBF) and ECochG potentials from the round window of rabbits in vivo. The microprobe is suitable for monitoring cochlear blood flow and auditory cochlear potentials during human surgery.

An ion microprobe study of the intra-crystalline behavior of REE and selected trace elements in pyroxene from mare basalts with different cooling and crystallization histories

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

Shearer, C.K.; Papike, J.J.; Simon, S.B.

1989-05-01

To study the effects of crystallization sequence and rate on trace element zoning characteristics of pyroxenes, the authors used combined electron microprobe-ion microprobe techniques on four nearly isochemical Apollo 12 and 15 pigeonite basalts with different cooling rates and crystallization histories. Major and minor element zoning characteristics are nearly identical to those reported in the literature. All the pyroxenes have similar chondrite-normalized REE patterns: negative Eu anomalies, positive slopes as defined by Yb/Ce, and slopes of REE patterns from Ce to Sm much steeper than from Gd to Yb. These trace element zoning characteristics in pyroxene and the partitioning ofmore » trace elements between pyroxene and the melt are intimately related to the interplay among the efficiency of the crystallization process, the kinetics at the crystal-melt interface, the kinetics of plagioclase nucleation and the characteristics of the crystal chemical substitutions within both the pyroxene and the associated crystallizing phases (i.e. plagioclase).« less

Rapid correction of electron microprobe data for multicomponent metallic systems

NASA Technical Reports Server (NTRS)

Gupta, K. P.; Sivakumar, R.

1973-01-01

This paper describes an empirical relation for the correction of electron microprobe data for multicomponent metallic systems. It evaluates the empirical correction parameter, a for each element in a binary alloy system using a modification of Colby's MAGIC III computer program and outlines a simple and quick way of correcting the probe data. This technique has been tested on a number of multicomponent metallic systems and the agreement with the results using theoretical expressions is found to be excellent. Limitations and suitability of this relation are discussed and a model calculation is also presented in the Appendix.

$ANBA; a rapid, combined data acquisition and correction program for the SEMQ electron microprobe

USGS Publications Warehouse

McGee, James J.

1983-01-01

$ANBA is a program developed for rapid data acquisition and correction on an automated SEMQ electron microprobe. The program provides increased analytical speed and reduced disk read/write operations compared with the manufacturer's software, resulting in a doubling of analytical throughput. In addition, the program provides enhanced analytical features such as averaging, rapid and compact data storage, and on-line plotting. The program is described with design philosophy, flow charts, variable names, a complete program listing, and system requirements. A complete operating example and notes to assist in running the program are included.

Micro-PIXE studies of Lupinus angustifolius L. after treatment of seeds with molybdenum

NASA Astrophysics Data System (ADS)

Przybylowicz, W. J.; Mesjasz-Przybylowicz, J.; Wouters, K.; Vlassak, K.; Combrink, N. J. J.

1997-02-01

An example of nuclear microprobe application in agriculture is presented. The NAC nuclear microprobe was used to determine quantitative elemental distribution of major, minor and trace elements in Lupinus angustifolius L. (Leguminosae) after treatment of seeds with molybdenum. Experiments were performed in order to establish safe concentration levels and sources of Mo in seed treatments. Elemental distributions in Mo-treated plants and in the non-treated control plants were studied in order to explain how Mo causes toxicity. Some specific regions of Mo and other main and trace elements enrichment were identified.

Use of an integrated approach to characterize the physicochemical properties of foundry green sands

USDA-ARS?s Scientific Manuscript database

A fresh green sand, spent green sand, and a weathered spent green sand from a landfill were analyzed using diffractometry, electron microscopy, granulometry, spectrometry, and thermogravimetry. Our objective was to understand how the physicochemical properties of the green sands change from their o...

San Francisco Estuary Striped Bass Migration History Determined by Electron-microprobe Analysis of Otolith Sr/Ca Ratio

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

Ostrach, D J; Phillis, C C; Weber, P K

2004-09-17

Habitat use has been shown to be an important factor in the bioaccumulation of contaminants in striped bass. This study examines migration in striped bass as part of a larger study investigating bioaccumulation and maternal transfer of xenobiotics to progeny in the San Francisco Estuary system. Habitat use, residence time and spawning migration over the life of females (n = 23) was studied. Female striped bass were collected between Knights Landing and Colusa on the Sacramento River during the spawning runs of 1999 and 2001. Otoliths were removed, processed and aged via otolith microstructure. Subsequently, otoliths were analyzed for strontium/calciummore » (Sr/Ca) ratio using an electron-microprobe to measure salinity exposure and to distinguish freshwater, estuary, and marine habitat use. Salinity exposure during the last year before capture was examined more closely for comparison of habitat use by the maternal parent to contaminant burden transferred to progeny. Results were selectively confirmed by ion microprobe analyses for habitat use. The Sr/Ca data demonstrate a wide range of migratory patterns. Age of initial ocean entry differs among individuals before returning to freshwater, presumably to spawn. Some fish reside in freshwater year-round, while others return to more saline habitats and make periodic migrations to freshwater. Frequency of habitat shifts and residence times differs among fish, as well as over the lifetime of individual fish. While at least one fish spent its final year in freshwater, the majority of spawning fish spent their final year in elevated salinity. However, not all fish migrated to freshwater to spawn in the previous year. Results from this investigation concerning migration history in striped bass can be combined with contaminant and histological developmental analyses to better understand the bioaccumulation of contaminants and the subsequent effects they and habitat use have on fish populations in the San Francisco Estuary system.« less

The petrogenesis of L-6 chondrites - Insights from the chemistry of minerals

NASA Technical Reports Server (NTRS)

Curtis, D. B.; Schmitt, R. A.

1979-01-01

Measurements of the major, minor and trace element abundances of the major minerals of the L-6 chondrites Alfianello, Colby (WI) and Leedey are used to investigate the formation mechanisms of L-6 chondrites. Electron microprobe analysis was performed on individual grains of each mineral, and separated minerals were analyzed by instrumental and radiochemical neutron activation analysis. The compositions of the three meteorites are observed to be generally uniform, however different abundances and distributions of rare earth elements and Co and Ni indicate that the meteorites have different petrogenetic histories. Alkali element distributions are found to be incompatible with internal equilibration of a closed system.

Copper, zinc, gallium and germanium distributions in taenite lamellae of iron meteorites and their importance for cooling rate estimations

NASA Astrophysics Data System (ADS)

Braun-Dullaeus, Karl-Ulrich; Traxel, Kurt

1995-02-01

One method forestimating cooling rates of meteorite parent bodies is to model measured nickel distributions in taenite lamellae of iron meteorites. Goldstein and Ogilvie ( Geochim. Cosmochim. Acta29, 893, 1965) and Rasmussen ( Icarus45, 564, 1981) developed techniques based on this idea to examine the cooling history in the temperature range between ˜700 and ˜400°C. As a result of Instrumental Neutron Activation Analysis (INAA) Rasmussen et al. ( Meteoritics23, 105, 1988) postulated that some trace elements would also be good cooling rate indicators. They argued that elements with distinct diffusion behavior are sensitive to different temperature ranges. The new Heidelberg proton microprobe uses the method of Proton Induced X-ray Emission (PIXE) for elemental analysis. This microprobe is an appropriate instrument to measure distributions of trace elements with a spatial resolution of 2 μm. We demonstrated on the iron meteorites Cape York (Agpalilik), Toluca and Odessa that the elements copper, zinc, gallium and germanium imitate the profiles of nickel in taenite lamella. The interpretation of the Zn, Ga and Ge profiles leads to the conclusion that these elements undergo diffusion mechanisms comparable to those of Ni. The numerical simulation of Cu distributions with a simplified model points out that little new information can be obtained about the cooling history of the meteorites by modelling Cu profiles. To simulate Zn, Ga or Ge distributions, the use of ternary phase diagrams is necessary.

Metamorphic reactions in ruby corundum amphibolite from the Chunky Gal Mountain mafic-ultramafic complex, Clay County, North Carolina

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

Ranson, W.A.; Garihan, J.M.; Ulmer, K.E.

1992-01-01

Amphibolite outcrops of unusual mineralogy within the Chunky Gal Mountain mafic-ultramafic complex display cm-scale rhythmic layers with moderate-steep dips. Layers are troctolitic, gabbroic, and anorthositic in composition, locally in contact with dunite of the Buck Creek ultramafic body. Meta-gabbroic layers contain striking bladed, emerald green amphibole as the chief mafic phase and relict bronzite with reacted margins. An additional major phase is plagioclase, [approximately]An 95 based on microprobe analysis. Ruby corundum is a minor (> 5%) constituent, which in some of the gabbroic rocks is mantled by a reaction rim of fibrolite. The clinoamphibole has optical properties resembling magnesio-cummingtonite: colorlessmore » to pale green in plane light with (+) sign and 2V = 60--70[degree]. However, microprobe analysis of the clinoamphibole indicates alumino-magnesio-hornblende. Although the texture of the bronzite shows that it is breaking down, it is clear that the clinoamphibole and corundum could not be the reaction products without the addition of Al, Ca, and Si in an aqueous fluid. Associated meta-troctolitic layers contain plagioclase and coarse, anhedral olivines displaying an inner corona of bladed orthopyroxene, rimmed by symplectite. The granulite facies reactions is: plagioclase + olivine = clinopyroxene + garnet. The mesoscopic-scale proximity of troctolitic and gabbroic rhythmic layers indicates both underwent granulite facies metamorphism. Retrogression to amphibolite grade is apparent only in the gabbroic layers, resulting in assemblages distinguished locally by abundant emerald green clinoamphibole and corundum porphyroblasts rimmed by fibrolite.« less

High resolution cathodoluminescence spectroscopy of carbonate cementation in Khurmala Formation (Paleocene-L. Eocene) from Iraqi Kurdistan Region, Northern Iraq

NASA Astrophysics Data System (ADS)

Omer, Muhamed F.; Omer, Dilshad; Zebari, Bahroz Gh.

2014-12-01

A combination of high resolution cathodoluminsecnce-spectroscopy (HRS-CL) with spatial electron microprobe analysis and optical microscopy is used to determine paragenesis and history of cementation in the limestones and dolostones of Khurmala Formation which is exposed in many parts of Northern Iraq. Khurmala Formation was subjected to different diagenetic processes such as micritization, compaction, dissolution, neomorphism, pyritization and cementation that occurred during marine to shallow burial stages and culminated during intermediate to deep burial later stages. Five dolomite textures are recognized and classified according to crystal size distribution and crystal-boundary shape. Dolomitization is closely associated with the development of secondary porosity that pre-and postdates dissolution and corrosion; meanwhile such porosity was not noticed in the associated limestones. Microprobe analysis revealed three types of cement, calcite, dolomite and ankerite which range in their luminescence from dull to bright. Cathodoluminescence study indicated four main texture generations. These are (1) unzoned microdolomite of planar and subhedral shape, with syntaxial rim cement of echinoderm that show dull to red luminescence, (2) equant calcite cements filling interparticle pores which shows dull luminescence and weak zonal growth, (3.1) homogenous intrinsic blue stoichiometric calcite with dull luminescence and without activators, (3.2) coarse blocky calcite cement with strong oscillatory zoning and bright orange luminescence which postdates other calcite cements, (4) ankerite cement with red to orange, non-luminescence growth zonation which is the last formed cement.

Petrochronology in constraining early Archean Earth processes and environments: Barberton greenstone belt, South Africa

NASA Astrophysics Data System (ADS)

Grosch, Eugene

2017-04-01

Analytical and petrological software developments over the past decade have seen rapid innovation in high-spatial resolution petrological techniques, for example, laser-ablation ICP-MS, secondary ion microprobe (SIMS, nano-SIMS), thermodynamic modelling and electron microprobe microscale mapping techniques (e.g. XMapTools). This presentation will focus on the application of petrochronology to ca. 3.55 to 3.33 billion-year-old metavolcanic and sedimentary rocks of the Onverwacht Group, shedding light on the earliest geologic evolution of the Paleoarchean Barberton greenstone belt (BGB) of South Africa. The field, scientific drilling and petrological research conducted over the past 8 years, aims to illustrate how: (a) LA-ICP-MS and SIMS U-Pb detrital zircon geochronology has helped identify the earliest tectono-sedimentary basin and sediment sources in the BGB, as well as reconstructing geodynamic processes as early as ca. 3.432 billion-years ago; (b) in-situ SIMS multiple sulphur isotope analysis of sulphides across various early Archean rock units help to reconstruct atmospheric, surface and subsurface environments on early Archean Earth and (c) the earliest candidate textural traces for subsurface microbial life can be investigated by in-situ LA-ICP-MS U-Pb dating of titanite, micro-XANES Fe-speciation analysis and metamorphic microscale mapping. Collectively, petrochronology combined with high-resolution field mapping studies, is a powerful multi-disciplinary approach towards deciphering petrogenetic and geodynamic processes preserved in the Paleoarchean Barberton greenstone belt of South Africa, with implications for early Archean Earth evolution.

Selective laser sintering of single-phase powder Cr-V tool steel

NASA Astrophysics Data System (ADS)

Kovalev, A. I.; Mishina, V. P.; Wainstein, D. L.; Titov, V. I.; Moiseev, V. F.; Tolochko, N. K.

2002-10-01

Presented is positive experience from selective laser sintering (SLS) of cylindrical steel specimens (3.0% C, 3.0% Cr, 1.0% Si, 12.0% V, Fe balance) 30 mm long and 5 mm in diameter by rapid prototyping. It was demonstrated that monolithic steel material could be successfully fabricated by this technology. Differential thermal analysis (DTA), scanning electron microscopy (SEM), and x-ray diffractometry (XRD) were used to study the microstructure, phase, and chemical composition of the source material and obtained specimens. Low-melting cementite-based eutectic was found to provide the liquid phase sintering of powder tool steel. The porosity of the green sintered specimens did not exceed 5%. The mean hardness value of sintered specimens was 825 HV.

Characterization of ALD grown TixAlyN and TixAlyC thin films

NASA Astrophysics Data System (ADS)

Kinnunen, S. A.; Malm, J.; Arstila, K.; Lahtinen, M.; Sajavaara, T.

2017-09-01

Atomic layer deposition (ALD) was used to grow TixAlyN and TixAlyC thin films using trimethylaluminum (TMA), titanium tetrachloride and ammonia as precursors. Deposition temperature was varied between 325 °C and 500 °C. Films were also annealed in vacuum and N2-atmosphere at 600-1000 °C. Wide range of characterization methods was used including time-of-flight elastic recoil detection analysis (ToF-ERDA), X-ray diffractometry (XRD), X-ray reflectometry (XRR), Raman spectroscopy, ellipsometry, helium ion microscopy (HIM), atomic force microscopy (AFM) and 4-point probe measurement for resistivity. Deposited films were roughly 100 nm thick and contained mainly desired elements. Carbon, chlorine and hydrogen were found to be the main impurities.

Clay-mineraloid weathering products in Antarctic meteorites

NASA Technical Reports Server (NTRS)

Gooding, James L.

1986-01-01

The production of clay mineraloids (CMs) in the weathering of stony meteorites recovered in the Allan Hills and Elephant Moraine areas of Antarctica is investigated, applying electron microbeam analysis, pyrolysis/mass spectroscopy, X-ray diffractometry, and differential scanning calorimetry to whole-rock chips from two eucrites, two diogenites, and an H5 chondrite. The data are presented in tables, graphs, and photomicrographs and characterized in detail. Massive to incipient-vermicular CM formations with smectitelike or micalike compositions and indications of poor crystallization are observed and attributed to hydrocryogenic diagenesis (with little or no liquid water) on time scales of 10-1000 kyr. The need to take the compositional effects of weathering into account before attempting to reconstruct the preterrestrial histories of meteorites is stressed.

Lattice distortion and strain relaxation in epitaxial thin films of multiferroic TbMnO3 probed by X-ray diffractometry and micro-Raman spectroscopy

NASA Astrophysics Data System (ADS)

Hu, Y.; Stender, D.; Medarde, M.; Lippert, T.; Wokaun, A.; Schneider, C. W.

2013-08-01

A detailed structural XRD analysis of (1 1 0)-oriented TbMnO3 thin films grown on (1 1 0)-YAlO3 substrates shows the co-existence of a strained and relaxed "sublayer" within the films due to strain relaxation during epitaxial growth by pulsed laser deposition. The substrate-film lattice mismatch yields a compressive strain anisotropy along the two in-plane directions, i.e. [1 -1 0] and [0 0 1] and a monoclinic distortion. A further manifestation of the growth-induced strain is the hardening of Raman active modes as a result of changed atomic motions along the [1 -1 0] and [0 0 1] directions.

Histological changes induced by 15 F CO2 laser microprobe especially designed for root canal sterilization: an in-vivo study

NASA Astrophysics Data System (ADS)

Kesler, Gavriel; Koren, Rumelia; Gal, Rivka

1998-04-01

Until now, no suitable delivery fiber existed for CO2 laser endodontic radiation in the apical region where it is most difficult to eliminate the pulp tissue using conventional methods. To overcome this problem, we designed a microprobe that reaches closer to the apex, distributing the energy density to a smaller area of the root canal, thus favorably increasing the thermal effects. The 15 F CO2 microprobe is a flexible, hollow, metal fiber, 300 micrometer in diameter and 20 mm in length, coupled onto a handpiece, with the following radiation parameters: wavelength -- 10.6 micrometer; pulse duration -- 50m/sec; energy per pulse 0.25 joule; energy density -- 353.7J/cm2 per pulse; power on tissue -- 5 W. The study was conducted on 30 vital maxillary or mandibulary; central, lateral, or premolar teeth destined for extraction due to periodontal problems. Twenty were experimentally treated with pulsed CO2 laser delivered by this newly developed fiber after conventional root canal preparation. Temperature measured at three points on the root surface during laser treatment did not exceed 38 degrees Celsius. Ten teeth represented the control group in which only root canal preparation was performed in the conventional method. Histological examination of the laser treated teeth showed coagulation necrosis and vacuolization of remaining pulp tissue in the root canal periphery. Primary and secondary dentin appeared normal, in all cases treated with 15 F CO2 laser. Gramm stain and bacteriologic examination revealed complete sterilization. These results demonstrate the unique capabilities of this special microprobe in sterilization of the root canal, and no thermal damage to the surrounding tissue.

Improved 206Pb/238U microprobe geochronology by the monitoring of a trace-element-related matrix effect; SHRIMP, ID-TIMS, ELA-ICP-MS and oxygen isotope documentation for a series of zircon standards

USGS Publications Warehouse

Black, L.P.; Kamo, S.L.; Allen, C.M.; Davis, D.W.; Aleinikoff, J.N.; Valley, J.W.; Mundil, R.; Campbell, I.H.; Korsch, R.J.; Williams, I.S.; Foudoulis, C.

2004-01-01

Precise isotope dilution-thermal ionisation mass spectrometry (ID-TIMS) documentation is given for two new Palaeozoic zircon standards (TEMORA 2 and R33). These data, in combination with results for previously documented standards (AS3, SL13, QGNG and TEMORA 1), provide the basis for a detailed investigation of inconsistencies in 206Pb/238U ages measured by microprobe. Although these ages are normally consistent between any two standards, their relative age offsets are often different from those established by ID-TIMS. This is true for both sensitive high-resolution ion-microprobe (SHRIMP) and excimer laser ablation-inductively coupled plasma-mass spectrometry (ELA-ICP-MS) dating, although the age offsets are in the opposite sense for the two techniques. Various factors have been investigated for possible correlations with age bias, in an attempt to resolve why the accuracy of the method is worse than the indicated precision. Crystallographic orientation, position on the grain-mount and oxygen isotopic composition are unrelated to the bias. There are, however, striking correlations between the 206Pb/238U age offsets and P, Sm and, most particularly, Nd abundances in the zircons. Although these are not believed to be the primary cause of this apparent matrix effect, they indicate that ionisation of 206Pb/238U is influenced, at least in part, by a combination of trace elements. Nd is sufficiently representative of the controlling trace elements that it provides a quantitative means of correcting for the microprobe age bias. This approach has the potential to reduce age biases associated with different techniques, different instrumentation and different standards within and between laboratories. Crown Copyright ?? 2004 Published by Elsevier B.V. All rights reserved.

Fracture resistance of dental nickel-titanium rotary instruments with novel surface treatment: Thin film metallic glass coating.

PubMed

Chi, Chih-Wen; Deng, Yu-Lun; Lee, Jyh-Wei; Lin, Chun-Pin

2017-05-01

Dental nickel-titanium (NiTi) rotary instruments are widely used in endodontic therapy because they are efficient with a higher success rate. However, an unpredictable fracture of instruments may happen due to the surface characteristics of imperfection (or irregularity). This study assessed whether a novel surface treatment could increase fatigue fracture resistance of dental NiTi rotary instruments. A 200- or 500-nm thick Ti-zirconium-boron (Ti-Zr-B) thin film metallic glass was deposited on ProTaper Universal F2 files using a physical vapor deposition process. The characteristics of coating were analyzed by scanning electron microscopy, transmission electron microscopy, and X-ray diffractometry. In cyclic fatigue tests, the files were performed in a simulated root canal (radius=5 mm, angulation=60°) under a rotating speed of 300rpm. The fatigue fractured cross sections of the files were analyzed with their fractographic performances through scanning electron microscopy images. The amorphous structure of the Ti-Zr-B coating was confirmed by transmission electron microscopy and X-ray diffractometry. The surface of treated files presented smooth morphologies without grinding irregularity. For the 200- and 500-nm surface treatment groups, the coated files exhibited higher resistance of cyclic fatigue than untreated files. In fractographic analysis, treated files showed significantly larger crack-initiation zone; however, no significant differences in the areas of fatigue propagation and catastrophic fracture were found compared to untreated files. The novel surface treatment of Ti-Zr-B thin film metallic glass on dental NiTi rotary files can effectively improve the fatigue fracture resistance by offering a smooth coated surface with amorphous microstructure. Copyright © 2016. Published by Elsevier B.V.

Optical, Fluorescence with quantum analysis of hydrazine (1, 3- Dinitro Phenyl) by DFT and Ab initio approach

NASA Astrophysics Data System (ADS)

Cecily Mary Glory, D.; Sambathkumar, K.; Madivanane, R.; Velmurugan, G.; Gayathri, R.; Nithiyanantham, S.; Venkatachalapathy, M.; Rajkamal, N.

2018-07-01

Experimental and computational study of molecular structure, vibrational and UV-spectral analysis of Hydrazine (1, 3- Dinitrophenyl) (HDP) derivatives. The crystal was grown by slow cooling method and the crystalline perfection of single crystals was evaluated by high resolution X-ray diffractometry (HRXRD) using a multicrystal X-ray diffractometer. Fluorescence, FT-IR and FT-Raman spectra of HDP crystal were recorded. The assignments of the vibrational spectra have been carried out with the help of normal co-ordinate analysis (NCA) followed by scaled quantum force field methodology (SQMFF). NMR studies have confirmed respectively the crystal structure and functional groups of the grown crystal. The energy and oscillator strength calculated by Time-Dependent Density Functional Theory (TD-DFT) result complements the experimental findings. The calculated MESP, UV, HOMO-LUMO energies show that charge transfer done within the molecule. And various thermodynamic parameters are studied. Fukui determines the local reactive site of electrophilic, nucleophilic, descriptor.

In situ removal of arsenic from groundwater by using permeable reactive barriers of organic matter/limestone/zero-valent iron mixtures.

PubMed

Gibert, O; de Pablo, J; Cortina, J-L; Ayora, C

2010-08-01

In this study, two mixtures of municipal compost, limestone and, optionally, zero-valent iron were assessed in two column experiments on acid mine treatment. The effluent solution was systematically analysed throughout the experiment and precipitates from both columns were withdrawn for scanning electron microscopy, energy-dispersive X-ray spectroscopy, X-ray diffractometry analysis and, from the column containing zero-valent iron, solid digestion and sequential extraction analysis. The results showed that waters were cleaned of arsenic, metals and acidity, but chemical and morphological analysis suggested that metal removal was not due predominantly to biogenic sulphide generation but to pH increase, i.e. metal (oxy)hydroxide and carbonate precipitation. Retained arsenic and metal removal were clearly associated to co-precipitation with and/or sorption on iron and aluminum (oxy)hydroxides. An improvement on the arsenic removal efficiency was achieved when the filling mixture contained zero-valent iron. Values of arsenic concentrations were then always below 10 microg/L.

Preliminary mineralogical data on epithermal ore veins associated with Rosia Poieni porphyry copper deposit, Apuseni Mountains, Romania

NASA Astrophysics Data System (ADS)

Iatan, E. L.; Popescu, Gh. C.

2012-04-01

Rosia Poieni is the largest porphyry copper (±Au±Mo) deposits associated with Neogene magmatic rocks from the South Apuseni Mountains, being located approximately 8 km northeast of the town of Abrud. During a recent examination of some epithermal mineralized veins, crosscutting the porphyry mineralization from the Roşia Poieni deposit, two species of tellurides and one tellurosulfide minerals were identified. The studied samples were collected from the + 1045 m level, SW side of the open pit and are represented by epithermal veins, crosscutting the porphyry copper mineralized body. The thickness of the veins is almost 4 cm. Following reflected-polarized light microscopy to identify the ore-mineral assemblages, the polished sections were studied with a Scanning Electron Microscope (SEM) equipped with a back-scattered electron (BSE) detector to study fine-sized minerals. Quantitative compositional data were determined using a Cameca SX 50 electron microprobe (EMP). Based on optical microscopy, SEM and EMPA three mineral associations have been separated inside the epithermal vein, from the margins to the centre: 1. quartz+tennantite-tetrahedrite+goldfieldite+pyrite+sphalerite; 2. quartz+pyrite+tellurobismutite; 3. chalcopyrite+hessite+vivianite. Goldfieldite occurs in anhedral grains and it is associated with tennantite-tetrahedrite and quartz. The electron microprobe analysis gave a variable content in Te between 13.28-13.39 wt.%, 43.34 wt.% Cu, 0.1 wt. % Fe, 0.2 wt.% Zn, 14.68 wt.% As, 4.35 wt.% Sb and 24.84 wt.% S. The calculated formula for the goldfieldite is Cu11.8Te1.8(Sb,As)4S13.4. The EPM analyses on tetrahedrite-tennantite revealed a low content in Te (0.02-0.03 wt.%) and 42.23 wt.% Cu, 2.67 wt.% Fe, 7.34 wt.% Zn, 0.04 wt.% Sb, 19.28 wt.% As and 28.4 wt.% S. The calculated formula is Cu9.8(Fe,Zn)2.4(Sb,As,Te)3.8S13. The variable ratio of the Te content may reflect a variable content of Te in the hydrothermal fluids from which the tellurian tetrahedrite precipitated. Hessite lies close to the grain boundary between the calchopyrite grains, which is associated with vivianite. Electron microprobe analysis gave 57.73 wt.% Ag and 42.27 wt.% Te with calculated stoichiometric formula Ag1.9Te1.1 . Tellurobismuthite it forms irregular grains and it is associated with quartz and pyrite. Electron microprobe analysis gave 57.20 wt.% Bi and 42.80 wt.% Te with calculated stoichiometric formula Bi2.2Te2.8. Based on the mineral assemblages separated inside the ore vein and on the ratio of the Te content for the different identified tellurium bearing minerals, we can conclude that the Te content of the fluids from which they precipitated, increased from the margins to the centre of the vein. In summary, this study of specimens from Rosia Poieni porphyry copper deposit, has resulted in the recognition of some tellurium-bearing minerals, not reported by previous workers. These minerals are represented by tellurobismutite, hessite and goldfieldite and they are associated with epithermal vein mineralization (pyrite, chalcopyrite, sphalerite, tennantite-tetrahedrite, quartz, vivianite). The presence of tellurium indicates the transition between porphyry-style mineralization to epithermal vein mineralization. Acknowledgements: This work was supported by the strategic grant POSDRU/89/1.5/S58852, Project "Postdoctoral program for training scientific researches" co-financed by the European Social Found within the Sectorial Operational Program Human Resources Development 2007-2013".

A High Resolution Microprobe Study of EETA79001 Lithology C

NASA Technical Reports Server (NTRS)

Schrader, Christian M.; Cohen, B. A.; Donovan, J. J.; Vicenzi, E. P.

2010-01-01

Antarctic meteorite EETA79001 has received substantial attention for possibly containing a component of Martian soil in its impact glass (Lithology C) [1]. The composition of Martian soil can illuminate near-surface processes such as impact gardening [2] and hydrothermal and volcanic activity [3,4]. Impact melts in meteorites represent our most direct samples of Martian regolith. We present the initial findings from a high-resolution electron microprobe study of Lithology C from Martian meteorite EETA79001. As this study develops we aim to extract details of a potential soil composition and to examine Martian surface processes using elemental ratios and correlations.

X-ray microprobe of orbital alignment in strong-field ionized atoms.

PubMed

Young, L; Arms, D A; Dufresne, E M; Dunford, R W; Ederer, D L; Höhr, C; Kanter, E P; Krässig, B; Landahl, E C; Peterson, E R; Rudati, J; Santra, R; Southworth, S H

2006-08-25

We have developed a synchrotron-based, time-resolved x-ray microprobe to investigate optical strong-field processes at intermediate intensities (10(14) - 10(15) W/cm2). This quantum-state specific probe has enabled the direct observation of orbital alignment in the residual ion produced by strong-field ionization of krypton atoms via resonant, polarized x-ray absorption. We found strong alignment to persist for a period long compared to the spin-orbit coupling time scale (6.2 fs). The observed degree of alignment can be explained by models that incorporate spin-orbit coupling. The methodology is applicable to a wide range of problems.

Electron microprobe evaluation of terrestrial basalts for whole-rock K-Ar dating

USGS Publications Warehouse

Mankinen, E.A.; Brent, Dalrymple G.

1972-01-01

Four basalt samples for whole-rock K-Ar dating were analyzed with an electron microprobe to locate potassium concentrations. Highest concentrations of potassium were found in those mineral phases which were the last to crystallize. The two reliable samples had potassium concentrated in fine-grained interstitial feldspar and along grain boundaries of earlier formed plagioclase crystals. The two unreliable samples had potassium concentrated in the glassy matrix, demonstrating the ineffectiveness of basaltic glass as a retainer of radiogenic argon. In selecting basalt samples for whole-rock K-Ar dating, particular emphasis should be placed on determining the nature and condition of the fine-grained interstitial phases. ?? 1972.

Study of the toughening mechanisms in bone and biomimetic hydroxyapatite materials using Raman microprobe spectroscopy.

PubMed

Pezzotti, Giuseppe; Sakakura, Seiji

2003-05-01

A Raman microprobe spectroscopy characterization of microscopic fracture mechanisms is presented for a natural hydroxyapatite material (cortical bovine femur) and two synthetic hydroxyapatite-based materials with biomimetic structures-a hydroxyapatite skeleton interpenetrated with a metallic (silver) or a polymeric (nylon-6) phase. In both the natural and synthetic materials, a conspicuous amount of toughening arose from a microscopic crack-bridging mechanism operated by elasto-plastic stretching of unbroken second-phase ligaments along the crack wake. This mechanism led to a rising R-curve behavior. An additional micromechanism, responsible for stress relaxation at the crack tip, was recognized in the natural bone material and was partly mimicked in the hydroxyapatite/silver composite. This crack-tip mechanism conspicuously enhanced the cortical bone material resistance to fracture initiation. A piezo-spectroscopic technique, based on a microprobe measurement of 980 cm(-1) Raman line of hydroxyapatite, enabled us to quantitatively assess in situ the microscopic stress fields developed during fracture both at the crack tip and along the crack wake. Using the Raman piezo-spectroscopy technique, toughening mechanisms were assessed quantitatively and rationally related to the macroscopic fracture characteristics of hydroxyapatite-based materials. Copyright 2003 Wiley Periodicals, Inc.

Recent optimization of the beam-optical characteristics of the 6 MV van de Graaff accelerator for high brightness beams at the iThemba LABS NMP facility

NASA Astrophysics Data System (ADS)

Conradie, J. L.; Eisa, M. E. M.; Celliers, P. J.; Delsink, J. L. G.; Fourie, D. T.; de Villiers, J. G.; Maine, P. M.; Springhorn, K. A.; Pineda-Vargas, C. A.

2005-04-01

With the aim of improving the reliability and stability of the beams delivered to the nuclear microprobe at iThemba LABS, as well as optimization of the beam characteristics along the van de Graaff accelerator beamlines in general, relevant modifications were implemented since the beginning of 2003. The design and layout of the beamlines were revised. The beam-optical characteristics through the accelerator, from the ion source up to the analysing magnet directly after the accelerator, were calculated and the design optimised, using the computer codes TRANSPORT, IGUN and TOSCA. The ion source characteristics and optimal operating conditions were determined on an ion source test bench. The measured optimal emittance for 90% of the beam intensity was about 50π mm mrad for an extraction voltage of 6 kV. These changes allow operation of the Nuclear Microprobe at proton energies in the range 1 MeV-4 MeV with beam intensities of tenths of a pA at the target surface. The capabilities of the nuclear microprobe facility were evaluated in the improved beamline, with particular emphasis to bio-medical samples.

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.

MORPH-I (Ver 1.0) a software package for the analysis of scanning electron micrograph (binary formatted) images for the assessment of the fractal dimension of enclosed pore surfaces

USGS Publications Warehouse

Mossotti, Victor G.; Eldeeb, A. Raouf; Oscarson, Robert

1998-01-01

MORPH-I is a set of C-language computer programs for the IBM PC and compatible minicomputers. The programs in MORPH-I are used for the fractal analysis of scanning electron microscope and electron microprobe images of pore profiles exposed in cross-section. The program isolates and traces the cross-sectional profiles of exposed pores and computes the Richardson fractal dimension for each pore. Other programs in the set provide for image calibration, display, and statistical analysis of the computed dimensions for highly complex porous materials. Requirements: IBM PC or compatible; minimum 640 K RAM; mathcoprocessor; SVGA graphics board providing mode 103 display.

Ion microprobe U-Pb dating and strontium isotope analysis of biogenic apatite

NASA Astrophysics Data System (ADS)

Sano, Y.; Toyoshima, K.; Takahata, N.; Shirai, K.

2012-12-01

Conodonts are micro-fossils chemically composed of apatite which occurred in the body of one animal. They are guide fossils to show formation ages of sedimentary sequences with the highest resolution [1] and good samples to verify the dating method. We developed the ion microprobe U-Pb dating of apatite [2] and applied the method to a Carboniferous conodont [3] by using a SHRIMP II installed at Department of Earth and Planetary Sciences, Hiroshima University. Recently we have developed the NanoSIMS U-Pb dating method and successfully measured the formation ages of monazite [4] and zircon [5] at Atmosphere and Ocean Research Institute, University of Tokyo. In this work we carried out the NanoSIMS U-Pb dating of biogenic apatite such as conodont. Since the spot size of NanoSIMS is smaller than SHRIMP II, it is easier to have multi-spots on the single fragment of biogenic apatite. Based on the isochron method of U-Pb system, we have calculated the formation ages. They are consistent with those in literature. In order to study the chemical evolution of ocean during the past 600 Million years, strontium isotopes (87Sr/86Sr) of fossil marine carbonate such as coral skeletons and foraminifera tests were measured and compiled [6]. However they are not robust when the age is older than 500Ma, partly due to post-depositional histories. Apatite is more stable and more resistant to the alteration than carbonate [7]. Recently we have developed the method of NanoSIMS strontium isotopic analysis of a fish otolith, which composed of aragonite [8]. In this work we carried out the strontium isotopic analysis of biogenic apatite. The advantage of the ion microprobe technique over the TIMS (thermal ionization mass spectrometer) and MC-ICP-MS (multi-collector inductively coupled argon plasma mass spectrometer) method is preservation of the important textural context and to provide an opportunity for other simultaneous analytical work with high spatial resolution. This is the case for the combination of U-Pb dating and strontium isotope analysis of biogenic apatite. This method may be useful to extract the information of the chemistry of Past ocean in future. [1] Sweet and Donoghue (2001) J. Paleont. 75, 1174-1184. [3] Sano et al., (1999) Chem. Geol. 153, 249-258. [3] Sano and Terada (2001) Geophys. Res. Lett. 28, 831-834. [4] Sano et al. (2006) Geochem. J. 40, 597-608. [5] Takahata et al. (2008) Gondwana Res. 14, 587-596. [6] Prokoph et al. (2008) Earth Sci. Rev. 87, 113-133. [7] Karhu and Epstein (1986) Geochim. Cosmochim. Acta 50, 1745-1756. [8] Sano et al. (2008) App. Geochem. 23, 2406-2413.

Aspects of the evolution of the West Antarctic margin of Gondwanaland

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

Grunow, A.M.

1989-01-01

A combination of paleomagnetism, structural field mapping, microprobe analysis, microfabric analysis and {sup 40}Ar/{sup 39}Ar geochronology was used to elucidate the history of the West Antarctic crustal block and the evolution of subduction complexes along the Scotia Ridge. West Antarctica is composed of four crustal blocks whose relationship to East Antarctica and to each other throughout the Phanerozoic is not well known. These blocks are: the Ellsworth-Whitmore Mountains (EWM); the Antarctic Peninsula (AP); Thurston Island (TI); Marie Byrd Land (MBL). Paleomagnetic sampling and analysis were conducted on rocks from the EWM and TI blocks in the hope of constraining themore » motion of these blocks and the opening history of the Weddell Sea. The paleomagnetic results suggest that the AP, EWM, and TI blocks have moved relative to East Antarctica prior to the mid-Cretaceous and that the main opening of the Weddell Sea was between the Early and mid-Cretaceous. Detailed field mapping was conducted on the subduction complexes of the Scotia Metamorphic Complex (SMC) on Smith Island and Elephant Island (Antarctica). Polyphase ductile deformation characterizes the Smith Island and Elephant Island tectonites. Microprobe analyses indicate that the blue amphiboles from both areas are primary crossite. Pressure-temperature estimates for Smith Island blueschist metamorphism are {approximately}350 C at 6-7 kbars. The {sup 40}Ar/{sup 39}Ar geochronology indicates a complex thermal evolution for the SMC. The north to south increase in intensity of deformation and metamorphism on Elephant Island corresponds to decrease in {sup 40}Ar/{sup 39}Ar age. Uplift of the Smith Island blueschists occurred since 47 Ma while most of the uplift on Elephant Island occurred since {approximately}102 Ma.« less

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.

Thermal stress cycling of GaAs solar cells

NASA Technical Reports Server (NTRS)

Francis, Robert W.

1987-01-01

Thermal stress cycling was performed on gallium arsenide solar cells to investigate their electrical, mechanical, and structural integrity. Cells were cycled under low Earth orbit (LEO) simulated temperature conditions in vacuum. Cell evaluations consisted of power output values, spectral response, optical microscopy and ion microprobe mass analysis, and depth profiles on both front surface inter-grid areas and metallization contact grid lines. Cells were examined for degradation after 500, 5,000, 10,000 and 15,245 thermal cycles. No indication of performance degradation was found for any vendor's cell lot.

Thermoelectric properties of n-type polycrystalline BixSb2-xTe3 alloys

NASA Technical Reports Server (NTRS)

Snyder, J.; Gerovac, N.; Caillat, T.

2002-01-01

(BixSbl-x)2Te3(.5 = x = .7) polycrystalline samples were synthesized using a combination of melting and powder metallurgy techniques. The samples were hot pressed in graphite dies and cut perpendicular and parallel to the pressing direction. Samples were examined by microprobe analysis to determine their atomic composition. The thermoelectric properties were measured at room temperature in both directions. These properties include Seebeck coefficient, thermal conductivity, electrical resistivity, and Hall effect. The thermoelectric figure-of-merit, ZT, was calculated fiom these properties.

Primary melt and fluid inclusions in regenerated crystals and phenocrysts of olivine from kimberlites of the Udachnaya-East Pipe, Yakutia: The problem of the kimberlite melt

NASA Astrophysics Data System (ADS)

Tomilenko, A. A.; Kuzmin, D. V.; Bul'bak, T. A.; Sobolev, N. V.

2017-08-01

The primary melt and fluid inclusions in regenerated zonal crystals of olivine and homogeneous phenocrysts of olivine from kimberlites of the Udachnaya-East pipe, were first studied by means of microthermometry, optic and scanning electron microscopy, electron and ion microprobe analysis (SIMS), inductively coupled plasma mass-spectrometry (ICP MSC), and Raman spectroscopy. It was established that olivine crystals were regenerated from silicate-carbonate melts at a temperature of 1100°C.

Chemistry and particle track studies of Apollo 14 glasses.

NASA Technical Reports Server (NTRS)

Glass, B. P.; Storzer, D.; Wagner, G. A.

1972-01-01

The abundance and the composition of Apollo 14 glasses have been studied. Glass particles were analyzed for Si, Ti, Al, Fe, Mn, Mg, Na, and K by electron microprobe analysis. The refractive indices of 26 particles were determined by the oil immersion method. Track analyses have been carried out in order to determine the uranium content and the radiation history of glass particles. The proper identification of galactic and solar flare nuclei tracks makes it possible to estimated residence times of the glass particles in the top layer of the lunar soil.

Extracellular proteins limit the dispersal of biogenic nanoparticles

USGS Publications Warehouse

Moreau, J.W.; Weber, P.K.; Martin, M.C.; Gilbert, B.; Hutcheon, I.D.; Banfield, J.F.

2007-01-01

High-spatial-resolution secondary ion microprobe spectrometry, synchrotron radiation-based Fourier-transform infrared spectroscopy, and polyacrylamide gel analysis demonstrated the intimate association of proteins with spheroidal aggregates of biogenic zinc sulfide nanocrystals, an example of extracellular biomineralization. Experiments involving synthetic zinc sulfide nanoparticles and representative amino acids indicated a driving role for cysteine in rapid nanoparticle aggregation. These findings suggest that microbially derived extracellular proteins can limit the dispersal of nanoparticulate metal-bearing phases, such as the mineral products of bioremediation, that may otherwise be transported away from their source by subsurface fluid flow.

PROGRESS ON THE STUDY OF THE URANIUM-ALUMINUM-IRON CONSTITUTION DIAGRAM FOR THE PERIOD SEPTEMBER 1-DECEMBER 31, 1963

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

Russell, R.B.

The U--Al--Fe constitution diagram up to about 1000 ppm each of aluminum and iron is sthdied. The techniques used for this study include optical, electron, and x-ray metallography; microprobe analysis, electric conductivity, and hardness measurements. A combination of techniques are giving evidence of the amount of solid solubility of aluminum and iron in alpha, beta, and gamma uranium at selected higher temperatures. The U-Al and U-Fe phase diagrams are also being determined. (N.W.R.)

The composition of coexisting jarosite-group minerals and water from the Richmond mine, Iron Mountain, California

USGS Publications Warehouse

Jamieson, Heather E.; Robinson, Clare; Alpers, Charles N.; Nordstrom, D. Kirk; Poustovetov, Alexei; Lowers, Heather A.

2005-01-01

Jarosite-group minerals accumulate in the form of stalactites and fine-grained mud on massive pyrite in the D drift of the Richmond mine, Iron Mountain, California. Water samples were collected by placing beakers under the dripping stalactites and by extracting pore water from the mud using a centrifuge. The water is rich in Fe3+ and SO4 2−, with a pH of approximately 2.1, which is significantly higher than the extremely acidic waters found elsewhere in the mine. Electron-microprobe analysis and X-ray mapping indicate that the small crystals (<10 μm in diameter) are compositionally zoned with respect to Na and K, and include hydronium jarosite corresponding to the formula (H3O)0.6K0.3Na0.1Fe3 3+(SO4)2(OH)6. The proton-microprobe analyses indicate that the jarosite-group minerals contain significant amounts of As, Pb and Zn, and minor levels of Bi, Rb, Sb, Se, Sn and Sr. Speciation modeling indicates that the drip waters are supersaturated with respect to jarosite-group minerals. The expected range in composition of jarosite-group solid-solution in equilibrium with the pore water extracted from the mud was found to be consistent with the observed range in composition.

Newly recognized hosts for uranium in the Hanford Site vadose zone

USGS Publications Warehouse

Stubbs, J.E.; Veblen, L.A.; Elbert, D.C.; Zachara, J.M.; Davis, J.A.; Veblen, D.R.

2009-01-01

Uranium contaminated sediments from the U.S. Department of Energy's Hanford Site have been investigated using electron microscopy. Six classes of solid hosts for uranium were identified. Preliminary sediment characterization was carried out using optical petrography, and electron microprobe analysis (EMPA) was used to locate materials that host uranium. All of the hosts are fine-grained and intergrown with other materials at spatial scales smaller than the analytical volume of the electron microprobe. A focused ion beam (FIB) was used to prepare electron-transparent specimens of each host for the transmission electron microscope (TEM). The hosts were identified as: (1) metatorbernite [Cu(UO2)2(PO4)2??8H2O]; (2) coatings on sediment clasts comprised mainly of phyllosilicates; (3) an amorphous zirconium (oxyhydr)oxide found in clast coatings; (4) amorphous and poorly crystalline materials that line voids within basalt lithic fragments; (5) amorphous palagonite surrounding fragments of basaltic glass; and (6) Fe- and Mn-oxides. These findings demonstrate the effectiveness of combining EMPA, FIB, and TEM to identify solid-phase contaminant hosts. Furthermore, they highlight the complexity of U geochemistry in the Hanford vadose zone, and illustrate the importance of microscopic transport in controlling the fate of contaminant metals in the environment. ?? 2008 Elsevier Ltd.

Determination of the chemical properties of residues retained in individual cloud droplets by XRF microprobe at SPring-8

NASA Astrophysics Data System (ADS)

Ma, C.-J.; Tohno, S.; Kasahara, M.; Hayakawa, S.

2004-06-01

To determine the chemical properties of residue retained in individual cloud droplets is primarily important for the understanding of rainout mechanism and aerosol modification in droplet. The sampling of individual cloud droplets were carried out on the summit of Mt. Taiko located in Tango peninsula, Kyoto prefecture, during Asian dust storm event in March of 2002. XRF microprobe system equipped at SPring-8, BL-37XU was applied to the subsequent quantification analysis of ultra trace elements in residues of individual cloud droplets. It was possible to form the replicas of separated individual cloud droplets on the thin collodion film. The two dimensional XRF maps for the residues in individual cloud droplets were clearly drawn by scanning of micro-beam. Also, XRF spectra of trace elements in residues were well resolved. From the XRF spectra for individual residues, the chemical mixed state of residues could be assumed. The chemical forms of Fe (Fe +++) and Zn (Zn +) could be clearly characterized by their K-edge micro-XANES spectra. By comparison of Z/Si mass ratios of residues in cloud droplets and those of the original sands collected in desert areas in China, the aging of ambient dust particles and their in cloud modification were indirectly assumed.

Investigation of Synthetic Mg(1.3)V(1.7)O4 Spinel with MgO Inclusions: Case Study of a Spinel with an Apparently occupied Interstitial Site

NASA Technical Reports Server (NTRS)

Uchida, Hinako; Righter, Kevin; Lavina, Barbara; Nowell, Matthew M.; Wright, Stuart I.; Downs, Robert T.; Yang, Hexiong

2007-01-01

A magnesium vanadate spinel crystal, ideally MgV2O4, synthesized at 1 bar, 1200 C and equilibrated under FMQ + 1.3 log f(sub o2) condition, was investigated using single-crystal X-ray diffraction, electron microprobe, and electron backscatter (EBSD). The initial X-ray structure refinements gave tetrahedral and octahedral site occupancies, along with the presence of 0.053 apfu Mg at an interstitial octahedral site . Back-scattered electron (BSE) images and electron microprobe analyses revealed the existence of an Mg-rich phase in the spinel matrix, which was too small (less than or equal to 3microns) for an accurate chemical determination. The EBSD analysis combined with X-ray energy dispersive spectroscop[y (XEDS) suggested that the Mg-rich inclusions are periclase oriented coherently with the spinel matrix. The final structure refinements were optimized by subtracting the X-ray intensity contributions (approx. 9%) of periclase reflections, which eliminated the interstitial Mg. This study provides insight into possible origins of refined interstitial cations reported in the the literature for spinel, and points to the difficulty of using only X-ray diffraction data to distinguish a spinel with interstitial cations from one with coherently oriented MgO inclusions.

Sudbury project (University of Muenster-Ontario Geological Survey): Petrology, chemistry, and origin of breccia formations

NASA Technical Reports Server (NTRS)

Stoeffler, D.; Deutsch, A.; Avermann, M.; Brockmeyer, P.; Lakomy, R.; Mueller-Mohr, V.

1992-01-01

Within the Sudbury Project of the University of Muenster and the Ontario Geological Survey special emphasis was put on the breccia formations exposed at the Sudbury structure (SS) because of their crucial role for the impact hypothesis. They were mapped and sampled in selected areas of the north, east, and south ranges of the SS. The relative stratigraphic positions of these units are summarized. Selected samples were analyzed by optical microscopy, SEM, microprobe, XRF and INAA, Rb-Sr and SM-Nd-isotope geochemistry, and carbon isotope analysis. The results of petrographic and chemical analysis for those stratigraphic units that were considered the main structural elements of a large impact basin are summarized.

Organic contamination analysis: High resolution mass spectrometric analysis of surface organics on selected areas of Surveyor 3

NASA Technical Reports Server (NTRS)

Simoneit, B. R.; Burlingame, A. L.

1972-01-01

The mirror and middle shroud were extracted for organics by washing the surfaces with solvents. The techniques are discussed. Ion microprobe analyses of the primarily atomic species are presented. The sources of the organic contaminants are: (1) hydrocarbons from lubricating oils and general terrestrial contamination, (2) dioctyl phthalate, probably from polyethylene bagging material (the plasticizer), (3) carboxylic acids from decomposition of grease and general terrestrial contamination, (4) silicones from sources such as lubricating oil, (5) outgassing of electronics and plasticizer, (6) vinyl alcohol and styrene copolymer, probably from electronic insulation, and (7) nitrogenous compounds from the lunar module and possibly Surveyor 3 engine exhaust.

New eutectic alloys and their heats of transformation

NASA Technical Reports Server (NTRS)

Farkas, D.; Birchenall, C. E.

1985-01-01

Eutectic compositions and congruently melting intermetallic compounds in binary and multicomponent systems among common elements such as Al, Ca, Cu, Mg, P, Si, and Zn may be useful for high temperature heat storage. In this work, heats of fusion of new multicomponent eutectics and intermetallic phases are reported, some of which are competitive with molten salts in heat storage density at high temperatures. The method used to determine unknown eutectic compositions combined results of differential thermal analysis, metallography, and microprobe analysis. The method allows determination of eutectic compositions in no more than three steps. The heats of fusion of the alloys were measured using commercial calorimeters, a differential thermal analyzer, and a differential scanning calorimeter.

Analysis of Short and Long Range Atomic Order in Nanocrystalline Diamonds with Application of Powder Diffractometry

NASA Technical Reports Server (NTRS)

Palosz, B.; Grzanka, E.; Stelmakh, S.; Pielaszek, R.; Bismayer, U.; Neuefiend, J.; Weber, H.-P.; Proffen, T.; VonDreele, R.; Palosz, W.;

Proteomic analysis of a rare urinary stone composed of calcium carbonate and calcium oxalate dihydrate: a case report.

PubMed

Kaneko, Kiyoko; Matsuta, Yosuke; Moriyama, Manabu; Yasuda, Makoto; Chishima, Noriharu; Yamaoka, Noriko; Fukuuchi, Tomoko; Miyazawa, Katsuhito; Suzuki, Koji

2014-03-01

The objective of the present study was to investigate the matrix protein of a rare urinary stone that contained calcium carbonate. A urinary stone was extracted from a 34-year-old male patient with metabolic alkalosis. After X-ray diffractometry and infrared analysis of the stone, proteomic analysis was carried out. The resulting mass spectra were evaluated with protein search software, and matrix proteins were identified. X-ray diffraction and infrared analysis confirmed that the stone contained calcium carbonate and calcium oxalate dihydrate. Of the identified 53 proteins, 24 have not been previously reported from calcium oxalate- or calcium phosphate-containing stones. The protease inhibitors and several proteins related to cell adhesion or the cytoskeleton were identified for the first time. We analyzed in detail a rare urinary stone composed of calcium carbonate and calcium oxalate dihydrate. Considering the formation of a calcium carbonate stone, the new identified proteins should play an important role on the urolithiasis process in alkaline condition. © 2013 The Japanese Urological Association.

X-Ray Diffraction of Intermetallic Compounds: A Physical Chemistry Laboratory Experiment

ERIC Educational Resources Information Center

Varberg, Thomas D.; Skakuj, Kacper

2015-01-01

Here we describe an experiment for the undergraduate physical chemistry laboratory in which students synthesize the intermetallic compounds AlNi and AlNi3 and study them by X-ray diffractometry. The compounds are synthesized in a simple one-step reaction occurring in the solid state. Powder X-ray diffractograms are recorded for the two compounds…

Selective removal of monoterpenes from bergamot oil by inclusion in deoxycholic acid.

PubMed

Fantin, Giancarlo; Fogagnolo, Marco; Maietti, Silvia; Rossetti, Stefano

2010-05-12

A new approach for removing monoterpenes (MTs) from bergamot oil by selective inclusion in deoxycholic acid (DCA) is proposed. The inclusion process is very efficient, the included fraction being composed mainly of limonene (71.7%) and gamma-terpinene (19.8%). On the other hand, the deterpenated bergamot oil fraction showed for the linalool and linalyl acetate derivatives significant increases from 16.6 and 21.4% to 18.3 and 42.2%, respectively. The major advantages of this methodology are its simplicity, the mild conditions employed, and the quantitative recovery of both host (DCA) and guest (monoterpenes) compounds. Differential scanning calorimetry (DSC), thermal gravimetry (TG), powder X-ray diffractometry (XRPD), infrared spectroscopy (IR), and proton magnetic resonance ((1)H NMR) analysis were used to investigate and characterize the inclusion compounds.

Marble protection: An inorganic electrokinetic approach

NASA Astrophysics Data System (ADS)

Meloni, Paola; Manca, Francesco; Carcangiu, Gianfranco

2013-05-01

The influence of an electric potential difference in an aqueous solution was studied as a method for depositing a calcium oxalate coating over a weathered carbonatic stone. Samples of weathered Carrara white marble were treated at 15 and 50 °C for 5 h in an electrokinetic cell, specifically conceived for this study, containing a solution of ammonium oxalate (4% by weight), and were subsequently characterised by scanning electron microscopy, X-ray diffractometry, thermogravimetric analysis and mercury intrusion porosimetry. The electrokinetic treatment proved to be a cost effective and time saving process, able to produce a thick and homogeneous calcium oxalate coating over the stone surface that improves its chemical and physical resistance in low pH environments, and is able to protect the stone from the by-products of urban pollution.

A facile and efficient strategy for the fabrication of porous linseed gum/cellulose superabsorbent hydrogels for water conservation.

PubMed

Zhang, Hao; Luan, Qian; Huang, Qingde; Tang, Hu; Huang, Fenghong; Li, Wenlin; Wan, Chuyun; Liu, Changsheng; Xu, Jiqu; Guo, Pingmei; Zhou, Qi

2017-02-10

The linseed gum/cellulose composite hydrogels were successfully fabricated by mixing cellulose and linseed gum solutions dissolved in the NaOH/urea aqueous system and cross-linked with epichlorohydrin. The morphology and structure of the composite hydrogels were investigated by scanning electron microscopy (SEM), Fourier transform infrared (FTIR) spectroscopy, X-ray diffractometry (XRD) and thermogravimetric analysis (TGA). The swelling ratio and water retention properties were investigated. The results revealed that linseed gum mainly contributed to water adsorption, whereas the cellulose acted as a backbone to strengthen the porous structure. This work provided a simple way to prepare cellulose-based superabsorbent hydrogels, which could be potentially applied as an effective water conservation material in agriculture. Copyright © 2016 Elsevier Ltd. All rights reserved.

Triaxial Measurement Method for Analysis of Residual Stress after High Feed Milling by X-Ray Diffraction

NASA Astrophysics Data System (ADS)

Čuma, Matúš; Török, Jozef; Telišková, Monika

2016-12-01

Surface integrity is a broad term which includes various quality factors affecting the functional properties of parts. Residual stress is one of these factors. Machining generates residual stresses in the surface and subsurface layers of the structural elements. X-ray diffractometry is a non-destructive method applicable for the measurement of residual stresses in surface and subsurface layers of components. The article is focused on the non-destructive progressive method of triaxial measurement of residual stress after machining the surface of sample by high feed milling technology. Significance of triaxial measuring is the capability of measuring in different angles so it is possible to acquire stress tensor containing normal and shear stress components acting in the spot of measuring, using a Cartesian coordinate system.

Evolution of Constitution, Structure, and Morphology in FeCo-Based Multicomponent Alloys

NASA Astrophysics Data System (ADS)

Li, R.; Stoica, M.; Liu, G.; Eckert, J.

2010-07-01

Constituent phases, melting behaviors, and microstructure of multicomponent (Fe0.5Co0.5) x (Mo0.1C0.2B0.5Si0.2)100- x alloys ( x = 95, 90, 85, 80, and 70) produced by copper mold casting were evaluated by various analysis techniques, i.e., X-ray diffractometry, scanning electronic microscopy with energy dispersive X-ray spectrometry, and differential scanning calorimetry. Metastable Fe3C- and Cr23C6-type phases were identified in the chill-cast alloys. A schematic illustration was proposed to explain the evolution of constituent phases and microstructure for the alloys with x = 95, 90, and 85 during the solidification process, which could be applicable to controlling microstructural formation of other multicomponent alloys with similar microstructures by artificially adjusting the composition.

Three-dimensional hydrogen microscopy using a high-energy proton probe

NASA Astrophysics Data System (ADS)

Dollinger, G.; Reichart, P.; Datzmann, G.; Hauptner, A.; Körner, H.-J.

2003-01-01

It is a challenge to measure two-dimensional or three-dimensional (3D) hydrogen profiles on a micrometer scale. Quantitative hydrogen analyses of micrometer resolution are demonstrated utilizing proton-proton scattering at a high-energy proton microprobe. It has more than an-order-of-magnitude better position resolution and in addition higher sensitivity than any other technique for 3D hydrogen analyses. This type of hydrogen imaging opens plenty room to characterize microstructured materials, and semiconductor devices or objects in microbiology. The first hydrogen image obtained with a 10 MeV proton microprobe shows the hydrogen distribution of the microcapillary system being present in the wing of a mayfly and demonstrates the potential of the method.

The Oxford scanning proton microprobe: A medical diagnostic application

NASA Astrophysics Data System (ADS)

Watt, F.; Grime, G. W.; Takacs, J.; Vaux, D. J. T.

1984-04-01

Primary biliary cirrhosis (PBC) is a disease characterised by progressive destruction of small intrahepatic bile ducts, cholestasis, and high levels of copper within the liver. The Oxford 1 μm scanning proton microprobe (SPM) has been used to construct elemental maps of a 7 μm section of diseased liver at several different magnifications. The results of these investigations have shown that the copper is distributed in small deposits ( < 5 μm) at specific locations in the liver. Further there appears to be a 1:1 atomic correlation between copper and sulphur, indicating the presence of an inorganic salt or a protein with approximately equal numbers of copper and sulphur atoms.

Micro Electron MicroProbe and Sample Analyzer

NASA Technical Reports Server (NTRS)

Manohara, Harish; Bearman, Gregory; Douglas, Susanne; Bronikowski, Michael; Urgiles, Eduardo; Kowalczyk, Robert; Bryson, Charles

2009-01-01

A proposed, low-power, backpack-sized instrument, denoted the micro electron microprobe and sample analyzer (MEMSA), would serve as a means of rapidly performing high-resolution microscopy and energy-dispersive x-ray spectroscopy (EDX) of soil, dust, and rock particles in the field. The MEMSA would be similar to an environmental scanning electron microscope (ESEM) but would be much smaller and designed specifically for field use in studying effects of geological alteration at the micrometer scale. Like an ESEM, the MEMSA could be used to examine uncoated, electrically nonconductive specimens. In addition to the difference in size, other significant differences between the MEMSA and an ESEM lie in the mode of scanning and the nature of the electron source.

Development of Ultra Low Temperature, Impact Resistant Lithium Battery for the Mars Microprobe

NASA Technical Reports Server (NTRS)

Frank, H.; Deligiannis, F.; Davies, E.; Ratnakumar, Bugga V.; Surampudi, S.; Russel, P. G.; Reddy, T. B.

1998-01-01

The requirements of the power source for the Mars Microprobe, to be backpacked on the Mars 98 Spacecraft, are fairly demanding, with survivability to a shock of the order of 80,000 g combined with an operational requirement at -80 C. Development of a suitable power system, based on primary lithium-thionyl chloride is underway for the last eighteen months, together with Yardney Technical Products Inc., Pawcatuck, CT. The battery consists of 4 cells of 2 Ah capacity at 25 C, of which at least 25 % would be available at -80 C, at a moderate rate of C/20. Each probe contains two batteries and two such probes will be deployed. The selected cell is designed around an approximate 1/2 "D" cells, with flat plate electrodes. Significant improvements to the conventional Li-SOCl2 cell include: (a) use of tetrachlorogallate salt instead of aluminate for improved low temperature performance and reduced voltage delay, (b) optimization of the salt concentration, and (c) modification of the cell design to develop shock resistance to 80,000 g. We report here results from our several electrical performance tests, mission simulation tests, microcalorimetry and AC impedance studies, and Air gun tests. The cells have successfully gone through mission-enabling survivability and performance tests for the Mars Microprobe penetrator.

Complementary microanalysis of Zn, Mn and Fe in the chelicera of spiders and scorpions using scanning MeV-ion and electron microprobes

NASA Astrophysics Data System (ADS)

Schofield, Robert; Lefevre, Harlan; Shaffer, Michael

1989-04-01

Energy-loss scanning transmission ion microscopy (ELSTIM or just STIM), PIXE and electron microprobe techniques are used to investigate certain minor element accumulations in a few spiders and scorpions. STIM and PIXE are used to survey the unsectioned specimens, while electron microprobe techniques are used for higher resolution investigations of several sections of the specimens. Concentration values measured using STIM and PIXE are found to be in satisfactory agreement with those measured using electron probe microanalysis. A garden spider Araneus diadematus is found to contain high concentrations of zinc in a thin layer near the surface of its fangs (reaching 23% of dry weight), and manganese in its marginal teeth (about 5% of dry weight). A wolf spider Alopecosa kochi is found to have similar concentrations of zinc in a layer near the surface of it's fang, and concentrations of manganese reaching 1.5% in a layer beneath the zinc containing layer. A scorpion Centruroides sp. is found to contain high concentrations of iron (reaching 8%) and zinc (reaching 24%) in the tips of teeth on the cheliceral fingers, and manganese (about 5%) in the stinger. The hypothesis that these elements simply harden the cuticle does not appear to explain their segregation patterns.

Flexible Microsensor Array for the Root Zone Monitoring of Porous Tube Plant Growth System

NASA Technical Reports Server (NTRS)

Sathyan, Sandeep; Kim, Chang-Soo; Porterfield, D. Marshall; Nagle, H. Troy; Brown, Christopher S.

2004-01-01

Control of oxygen and water in the root zone is vital to support plant growth in the microgravity environment. The ability to control these sometimes opposing parameters in the root zone is dependent upon the availability of sensors to detect these elements and provide feedback for control systems. In the present study we demonstrate the feasibility of using microsensor arrays on a flexible substrate for dissolved oxygen detection, and a 4-point impedance microprobe for surface wetness detection on the surface of a porous tube (PT) nutrient delivery system. The oxygen microsensor reported surface oxygen concentrations that correlated with the oxygen concentrations of the solution inside the PT when operated at positive pressures. At negative pressures the microsensor shows convergence to zero saturation (2.2 micro mol/L) values due to inadequate water film formation on porous tube surface. The 4-point microprobe is useful as a wetness detector as it provides a clear differentiation between dry and wet surfaces. The unique features of the dissolved oxygen microsensor array and 4-point microprobe include small and simple design, flexibility and multipoint sensing. The demonstrated technology is anticipated to provide low cost, and highly reliable sensor feedback monitoring plant growth nutrient delivery system in both terrestrial and microgravity environments.

X-ray microprobe synchroton radiation X-ray fluorescence application on human teeth of renal insufficiency patients

NASA Astrophysics Data System (ADS)

Marques, A. F.; Marques, J. P.; Casaca, C.; Carvalho, M. L.

2004-10-01

This work reports on the measurements of elemental profiles in teeth collected from patients with renal insufficiency. Elemental concentrations of Ti, Mn, Fe, Co, Ni, Cu, Zn, Se, Br, Rb Sr and Pb in different parts of teeth from patients with renal insufficiency are discussed and correlated with the corresponding values for healthy citizens. Both situations, patients with and without dialysis treatment were studied. The purpose of this work is to point out the influence of renal insufficiency together with long dialysis treatment, on teeth elemental content. An X-ray fluorescence set-up with microprobe capabilities, installed at the LURE synchrotron (France) was used for elemental determination. The resolution of the synchrotron microprobe was 100 μm and the energy of the incident photons was 19 keV. Teeth of citizens with renal insufficiency and those submitted since several years to dialysis treatment show a similar concentration with teeth of healthy subjects in what concerns the elemental distribution for Mn, Fe, Cu, Zn and Sr. However, higher levels of Pb were found in pulp region of diseased citizens when compared to values of healthy people. Very low concentrations of Ti, Co, Ni, Se, Br and Rb were found in all the analysed teeth. No difference was found in patients with and without dialysis treatment.

Tunable lasers and their application in analytical chemistry

NASA Technical Reports Server (NTRS)

Steinfeld, J. I.

1975-01-01

The impact that laser techniques might have in chemical analysis is examined. Absorption, scattering, and heterodyne detection is considered. Particular emphasis is placed on the advantages of using frequency-tunable sources, and dye solution lasers are regarded as the outstanding example of this type of laser. Types of spectroscopy that can be carried out with lasers are discussed along with the ultimate sensitivity or minimum detectable concentration of molecules that can be achieved with each method. Analytical applications include laser microprobe analysis, remote sensing and instrumental methods such as laser-Raman spectroscopy, atomic absorption/fluorescence spectrometry, fluorescence assay techniques, optoacoustic spectroscopy, and polarization measurements. The application of lasers to spectroscopic methods of analysis would seem to be a rewarding field both for research in analytical chemistry and for investments in instrument manufacturing.

Testing Mechanisms and Scales of Equilibrium Using Textural and Compositional Analysis of Porphyroblasts in Rocks with Heterogeneous Garnet Distributions

NASA Astrophysics Data System (ADS)

Ruthven, R. C.; Ketcham, R. A.; Kelly, E. D.

2015-12-01

Three-dimensional textural analysis of garnet porphyroblasts and electron microprobe analyses can, in concert, be used to pose novel tests that challenge and ultimately increase our understanding of metamorphic crystallization mechanisms. Statistical analysis of high-resolution X-ray computed tomography (CT) data of garnet porphyroblasts tells us the degree of ordering or randomness of garnets, which can be used to distinguish the rate-limiting factors behind their nucleation and growth. Electron microprobe data for cores, rims, and core-to-rim traverses are used as proxies to ascertain porphyroblast nucleation and growth rates, and the evolution of sample composition during crystallization. MnO concentrations in garnet cores serve as a proxy for the relative timing of nucleation, and rim concentrations test the hypothesis that MnO is in equilibrium sample-wide during the final stages of crystallization, and that concentrations have not been greatly altered by intracrystalline diffusion. Crystal size distributions combined with compositional data can be used to quantify the evolution of nucleation rates and sample composition during crystallization. This study focuses on quartzite schists from the Picuris Mountains with heterogeneous garnet distributions consisting of dense and sparse layers. 3D data shows that the sparse layers have smaller, less euhedral garnets, and petrographic observations show that sparse layers have more quartz and less mica than dense layers. Previous studies on rocks with homogeneously distributed garnet have shown that crystallization rates are diffusion-controlled, meaning that they are limited by diffusion of nutrients to growth and nucleation sites. This research extends this analysis to heterogeneous rocks to determine nucleation and growth rates, and test the assumption of rock-wide equilibrium for some major elements, among a set of compositionally distinct domains evolving in mm- to cm-scale proximity under identical P-T conditions.

Long-term clinical evaluation of endodontically treated teeth by 15 F CO2 laser microprobe: three years clinical follow-up of 1512 root canals--in-vivo study

NASA Astrophysics Data System (ADS)

Kesler, Gavriel; Koren, Rumelia; Kesler, Anat; Hay, Nissim; Gal, Rivka

1999-05-01

The purpose of this study was to determine the efficiency of 15 F CO2 laser microprobe, in cases of periapical lesions, by eliminating the pathological reaction caused by certain species of bacteria, reduction of reinfection and stimulation of osteogenesis in the periapical region. Until now, no suitable delivery fiber existed for CO2 laser endodontic radiation in the apical region where it is most difficult to eliminate the pulp tissue using conventional methods. To overcome this problem, Sharplan laser designed a microprobe that reaches closer to the apex, distributing the energy density to a smaller area of the root canal, thus favorably increasing the thermal effects. The study was conducted on 900 teeth, divided in two groups. 468 were new case, carefully selected according to strict parameters such as: wide periapical translucency over 1mm, supported by digital x-ray, with a lesion of 3mm and more. All root canals were mechanically prepared in the conventional method up to size 35, Physiological saline solution served as finding solution and were treated by 15 F CO2 laser microprobe for 60 pulses repeatedly. The temperature at the surrounding tissue of the root did not exceed 38 degrees C filling of the canal was possible at the same appointment, without antibiotical treatment. 432 of the cases, which were referred to us by other dentists, after an unsuccessful treatment according to the classical therapy, were treated by the same laser therapy. Follow up was performed by clinical examination, and digital x-ray taken, during and after treatment as well as after 3, 6, 9, 12 month. The result demonstrate 98% success rate in both study groups, according to objective criteria for a successful treatment such as: reduction of apical translucency after 2- 6 months, freedom form clinical complains, and no need for periapical surgery.

Chemical compositions, infrared spectroscopy, and X-ray diffractometry study on brown-rotted woods

Treesearch

Gai-Yun Li; Luo-Hua Huang; Chung Hse; Te-Fu Qin

2011-01-01

The effect of brown-rot decay on the chemical composition and crystallinity of Masson pine was studied by exposing it to Wolfiporia cocos (Schwein.) Ryvarden and Gilbn. for durations of up to 15 weeks in the field. The holocellulose content, α-cellulose content, and wood crystallinity decreased slowly in the initial stage, followed by a significant reduction...

X-Ray Microanalytic Concentration Measurements in Unsectioned Specimens: a Technique and its Application to Zinc, Manganese, and Iron Enriched Mechanical Structures of Organisms from Three Phyla

NASA Astrophysics Data System (ADS)

Schofield, Robert M. S.

A method for measuring concentrations of minor elements in microscopic volumes of heterogeneous, unsectioned biological specimens using an ion microprobe is developed. The element quantity is obtained from PIXE (Proton Induced X-ray Emission) and the total quantity of material is derived from STIM (Scanning Transmission Ion Microscopy) energy loss measurements. Sources of error, including changes in x-ray production cross section with proton energy and absorption of induced x-rays, are discussed and a method of calculating the total measurement uncertainty, typically about 25% here, is developed. The measurement accuracy is shown to be improved for symmetric specimens, and a method of using the bremsstrahlung background to correct for x-ray attenuation within irregular specimens is developed. Methods for measuring local concentrations in internal features are also discussed. With this technique, scorpions were found to contain cuticular accumulations of one or more heavy metals (manganese up to 5% of dry weight, iron up to 8%, zinc up to 24%) in the chelicera, pedipalp denticles, tarsal claws, and stingers; different region soften contained different metals. The stingers are argued to be of particular interest because they are not homologous to legs. Similar accumulations were found in spiders, some other chelicerates and crustaceans. Previous reports of manganese and zinc accumulations in insect and worm mouth parts were augmented with local concentration measurements and with the detection of other enrichment features (such as 6% iron in the paragnaths of the worm Nereis vexillosa). Zinc accumulations (up to only 0.1%) were also found in the tips of the teeth of a hagfish, Myxine + glutinosa. X-ray images of several of these features are presented. It is argued that the extreme magnitude of some concentration values suggests that some metals are incorporated in unusual biominerals rather than organically bound. Results of x-ray diffractometry and Vickers microhardness measurements are reported although the results are inconclusive. The atomic ratio of zinc to chlorine in these accumulations is shown not to be constant. It is suggested from their typical locations that at least two of the observed accumulation patterns impart different mechanical properties to the cuticle.

Tri-functional Fe2O3-encased Ag-doped ZnO nanoframework: magnetically retrievable antimicrobial photocatalyst

NASA Astrophysics Data System (ADS)

Karunakaran, Chockalingam; Vinayagamoorthy, Pazhamalai

2016-11-01

Fe2O3-encased ZnO nanoframework was obtained by hydrothermal method and was doped with Ag through photoreduction process. Energy dispersive x-ray spectroscopy, transmission electron microscopy (TEM), high resolution TEM, selected area electron diffractometry, x-ray diffractometry and Raman spectroscopy were employed for the structural characterization of the synthesized material. While the charge transfer resistance of the prepared nanomaterial is larger than those of Fe2O3 and ZnO the coercivity of the nanocomposite is less than that of hydrothermally obtained Fe2O3 nanostructures. Although Fe2O3/Ag-ZnO exhibits weak visible light absorption its band gap energy does not differ from that of ZnO. The photoluminescence of the fabricated nanoframework is similar to that of ZnO. The radiative recombination of charge carriers is slightly slower in Fe2O3/Ag-ZnO than in ZnO. The synthesized Fe2O3-encased Ag-doped ZnO, under UV A light, exhibits sustainable photocatalytic activity to degrade dye and is magnetically recoverable. Also, the Fe2O3/Ag-ZnO nanocomposite disinfects bacteria effectively in absence of direct illumination.

Petrology and Mineral Chemistry of New Olivine-Phyric Shergottite RBT04262

NASA Technical Reports Server (NTRS)

Dalton, H. A.; Peslier, A. H.; Brandon, A. D.; Lee, C.-T. A.; Lapen, T. J.

2008-01-01

RBT04262 was found by the 2004-2005 ANSMET team at the Roberts Massif in Antarctica. It is paired with RBT04261 and is classified as an olivine-phyric shergottite. RBT04261 is 4.0 x 3.5 x 2.5 cm and 78.8 g, and RBT04262 is 6.5 x 5.5 x 3.5 cm and 204.6 g. Both were partially covered by a fusion crust [1]. Chemical analysis and mapping of this meteorite was performed using the Cameca SX100 electron microprobe at NASA Johnson Space Center.

An occurrence of metastable cristobalite in high-pressure garnet Granulite

USGS Publications Warehouse

Darling, R.S.; Chou, I.-Ming; Bodnar, R.J.

1997-01-01

High-pressure (0.8 gigapascals) granulite facies garnet from Gore Mountain, New York, hosts multiple solid inclusions containing the low- pressure silica polymorph cristobalite along with albite and minor ilmenite. Identification of cristobalite is based on Raman spectra, electron microprobe analysis, and microthermometric measurements on the ??/?? phase transformation. The cristobalite plus albite inclusions may have originated as small, trapped samples of hydrous sodium-aluminum-siliceous melt. Diffusive loss of water from these inclusions under isothermal, isochoric conditions may have resulted in a large enough internal pressure decrease to promote the metastable crystallization of cristobalite.

Oxidation of silicon nitride sintered with rare-earth oxide additions

NASA Technical Reports Server (NTRS)

Mieskowski, D. M.; Sanders, W. A.

1985-01-01

The effects of rare-earth oxide additions on the oxidation of sintered Si3N4 were examined. Insignificant oxidation occurred at 700 and 1000 C, with no evidence of phase instability. At 1370 C, the oxidation rate was lowest for Y2O3 and increased for additions of La2O3, Sm2O3, and CeO2, in that order. Data obtained from X-ray diffraction, electron microprobe analysis, and scanning electron microscopy indicate that oxidation occurs via diffusion of cationic species from Si3N4 grain boundaries.

Quantitation of polymorphic impurity in entecavir polymorphic mixtures using powder X-ray diffractometry and Raman spectroscopy.

PubMed

Kang, Yanlei; Shao, Zhanying; Wang, Qiang; Hu, Xiurong; Yu, Dongdong

2018-05-26

Entecavir was used for the treatment of chronic hepatitis B through inhibiting hepatitis B virus. The anhydrous form of entecavir (ENT-A) often appeared as impurity polymorph in the manufacturing process of entecavir monohydrate (ENT-H) such as granulation, drying and compression. Since different crystal forms might affect drug bioavailability and therapeutic effect, it was vital to control the ENT-A content of the drug product. The work aimed to develop useful methods to assess ENT-A weight percentage in ENT-H. Powder X-ray diffractometry (PXRD) and Raman spectrometric methods were applied. Binary mixtures with different ratios of pure ENT-H and pure ENT-A were scanned using PXRD and Raman to obtain spectra. Then peak heights and peak areas versus weight percentage were used to construct calibration curves. The best linear regression analysis data for PXRD and Raman method were found to be R 2  = 0.9923 and R 2  = 0.9953, in the weight ratio range of 2.1-20.2% w/w% of ENT-A in binary mixtures. Limit of detection (LOD) of ENT-A was 0.38% and limit of quantitation (LOQ) was 1.15% for PXRD method. LOD and LOQ for Raman method were 0.48% and 1.16%. The results showed that PXRD and Raman methods: both were precise and accurate, and could be used for measurement of ENT-A content in the selected weight percentage range. Partial least squares (PLS) algorithm with four data pre-processing methods: including multiplicative scatter correlation (MSC), standard normal variate (SNV), first and second derivatives were applied and evaluated using prediction errors. The best performance of PLS was R 2  = 0.9958 with RMSEC (0.44%) and RMSEP (0.65%). Multivariate analysis for Raman spectra showed similar good results with univariate analysis, and would be an advantageous method when there were overlapped peaks in the spectra. In summary, the proposed PXRD and Raman method could be developed for the quality control of ENT-H. And Raman was a more promising method in industrial practice due to its slightly better precision, accuracy and time-saving advantage. Copyright © 2018 Elsevier B.V. All rights reserved.

Effect of peptidase inhibition on the pattern of intraspinally released immunoreactive substance P detected with antibody microprobes.

PubMed

Duggan, A W; Schaible, H G; Hope, P J; Lang, C W

1992-05-08

Antibody microprobes bearing antibodies to the C-terminus of substance P (SP) were used to measure release of immunoreactive (ir) SP in the dorsal horn of barbiturate anaesthetized spinal cats. Electrical stimulation of unmyelinated primary afferents of the ipsilateral tibial nerve produced a relatively localised release of ir SP in the superficial dorsal horn. Prior microinjection of the peptidase inhibitors kelatorphan and enalaprilat in the dorsal horn resulted in ir SP being detected over the whole of the dorsal horn and the overlying dorsal column. This pattern had previously been observed with evoked release of ir neurokinin A and supports the proposal that a slow degradation results in a neuropeptide accessing many sites remote from sites of release.

The Amsterdam quintuplet nuclear microprobe

NASA Astrophysics Data System (ADS)

van den Putte, M. J. J.; van den Brand, J. F. J.; Jamieson, D. N.; Rout, B.; Szymanski, R.

2003-09-01

A new nuclear microprobe comprising of a quintuplet lens system is being constructed at the Ion Beam Facility of the "Vrije Universiteit" Amsterdam in collaboration with the Microanalytical Research Centre of the University of Melbourne. An overview of the Amsterdam set-up will be presented. Detailed characterisation of the individual lenses was performed with the grid shadow method using a 2000 mesh Cu grid mounted at a relative angle of 0.5° to the vertical lens line focus. The lenses were found to have very low parasitic aberrations equal or below the minimum detectable limit for the method, which was approximately 0.1% for the sextupole component and 0.2% for the octupole component. We present experimental and theoretical grid shadow patterns, showing results for all five lenses.

Reliability design and assessment of a micro-probe using the results of a tensile test of a beryllium-copper alloy thin film

NASA Astrophysics Data System (ADS)

Park, Jun-Hyub; Shin, Myung-Soo

2011-09-01

This paper describes the results of tensile tests for a beryllium-copper (BeCu) alloy thin film and the application of the results to the design of a probe. The copper alloy films were fabricated by electroplating. To obtain the tensile characteristics of the film, the dog-bone type specimen was fabricated by the etching method. The tensile tests were performed with the specimen using a test machine developed by the authors. The BeCu alloy has an elastic modulus of 119 GPa and the 0.2% offset yield and ultimate tensile strengths of 1078 MPa and 1108 MPa, respectively. The design and manufacture of a smaller probe require higher pad density and smaller pad-pitch chips. It should be effective in high-frequency testing. For the design of a new micro-probe, we investigated several design parameters that may cause problems, such as the contact force and life, using the tensile properties and the design of experiment method in conjunction with finite element analysis. The optimal dimensions of the probe were found using the response surface method. The probe with optimal dimensions was manufactured by a precision press process. It was verified that the manufactured probe satisfied the life, the contact force and the over drive through the compression tests and the life tests of the probes.

The external scanning proton microprobe of Firenze: A comprehensive description

NASA Astrophysics Data System (ADS)

Giuntini, L.; Massi, M.; Calusi, S.

2007-06-01

An external proton scanning microbeam setup is installed on the -30° line of the new 3 MV tandem accelerator in Firenze; the most relevant features of the line, such as detection setup for IBA measurements, target viewing system, beam diagnostic and transport are described here. With our facility we can work with a beam spot on sample better than 10 μm full-width half-maximum (FWHM) and an intensity of some nanoamperes. Standard beam exit windows are silicon nitride (Si 3N 4) TEM membranes, 100 nm thick and 0.5×0.5 mm 2 wide; we also successfully performed measurements using membranes 1×1 mm 2 wide, 100 nm thick, and 2×2 mm 2 wide, 200 and 500 nm thick. Exploiting the yield of Si X-rays produced by the beam in the exit window as an indirect measurement of the charge, a beam charge monitor system was implemented. The analytical capabilities of the microbeam have been extended by integrating a two-detector PIXE setup with BS and PIGE detectors; the external scanning proton microprobe in Firenze is thus a powerful instrument to fully characterize samples by ion beam analysis, through the simultaneous collection of PIXE, PIGE and BS elemental maps. Its characteristics can make it often competitive with traditional in vacuum microbeam for measurements of thick targets.

Photoluminescent properties of complex metal oxide nanopowders for gas sensing

NASA Astrophysics Data System (ADS)

Bovhyra, R. V.; Mudry, S. I.; Popovych, D. I.; Savka, S. S.; Serednytski, A. S.; Venhryn, Yu. I.

2018-03-01

This work carried out research on the features of photoluminescence of the mixed and complex metal oxide nanopowders (ZnO/TiO2, ZnO/SnO2, Zn2SiO4) in vacuum and gaseous ambient. The nanopowders were obtained using pulsed laser reactive technology. The synthesized nanoparticles were characterized by X-ray diffractometry, energy-dispersive X-ray analysis, and scanning and transmission electron microscopy analysis for their sizes, shapes and collocation. The influence of gas environment on the photoluminescence intensity was investigated. A change of ambient gas composition leads to a rather significant change in the intensity of the photoluminescence spectrum and its deformation. The most significant changes in the photoluminescent spectrum were observed for mixed ZnO/TiO2 nanopowders. This obviously is the result of a redistribution of existing centers of luminescence and the appearance of new adsorption centers of luminescence on the surface of nanopowders. The investigated nanopowders can be effectively used as sensing materials for the construction of the multi-component photoluminescent sensing matrix.

Hierarchical macro-mesoporous structures in the system TiO{sub 2}-Al{sub 2}O{sub 3}, obtained by hydrothermal synthesis using Tween-20 as a directing agent

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

Garcia-Benjume, M.L.; Espitia-Cabrera, M.I.; Contreras-Garcia, M.E., E-mail: eucontre@zeus.umich.mx

2009-12-15

Macro-mesoporous powders of titania, alumina, and mixed titania-20%alumina systems were obtained by hydrothermal synthesis employing surfactant Tween-20 as structural directing agent in order to promote the textural properties of titania. The effect of the alumina in the titania phase and on textural properties was analyzed. The obtained powders presented a macroporous channel structure that was characterized by X-ray diffractometry, scanning and transmission electron microscopy, N{sub 2} adsorption-desorption analysis, pore size distribution, Fourier transform infrared spectrometry, and thermogravimetric analysis. It was found that alumina content retarded the anatase phase crystallization and increased the Brunauer-Emmet-Teller surface area from 136 to 210 m{supmore » 2}/g. The powders calcined at 400 deg. C are thermally stable and possess an interconnected macro-mesoporous hierarchical structure; the results indicate that this synthesis can be employed to prepare mixed titania-alumina with good textural properties.« less

Misfit strain relaxation in (Ba0.60Sr0.40)TiO3 epitaxial thin films on orthorhombic NdGaO3 substrates

NASA Astrophysics Data System (ADS)

Simon, W. K.; Akdogan, E. K.; Safari, A.

2006-07-01

Strain relaxation in (Ba0.60Sr0.40)TiO3 (BST) thin films on ⟨110⟩ orthorhombic NdGaO3 substrates is investigated by x-ray diffractometry. Pole figure analysis indicates a [010]BST∥[1¯10]NGO and [001]BST∥[001]NGO in-plane and [100]BST∥[100]NGO out-of-plane epitaxial relationship. The residual strains are relaxed at h ˜200nm, and for h >600nm, films are essentially strain free. Two independent dislocations mechanisms operate to relieve the anisotropic misfit strains along the principal directions. The critical thickness for misfit dislocation formation along [001] and [010] are 11 and 15nm, respectively. Stress analysis indicates deviation from linear elasticity for h <200. The films with 10

Distribution of siderophile and other trace elements in melt rock at the Chicxulub impact structure

NASA Technical Reports Server (NTRS)

Schuraytz, B. C.; Lindstrom, D. J.; Martinez, R. R.; Sharpton, V. L.; Marin, L. E.

1994-01-01

Recent isotopic and mineralogical studies have demonstrated a temporal and chemical link between the Chicxulub multiring impact basin and ejecta at the Cretaceous-Tertiary boundary. A fundamental problem yet to be resolved, however, is identification of the projectile responsible for this cataclysmic event. Drill core samples of impact melt rock from the Chichxulub structure contain Ir and Os abundances and Re-Os isotopic ratios indicating the presence of up to approx. 3 percent meteoritic material. We have used a technique involving microdrilling and high sensitivity instrumental neutron activation analysis (INAA) in conjunction with electron microprobe analysis to characterize further the distribution of siderophile and other trace elements among phases within the C1-N10 melt rock.

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

Reusch, L. M., E-mail: lmmcguire@wisc.edu; Den Hartog, D. J.; Goetz, J.

The two-color soft x-ray (SXR) tomography diagnostic on the Madison Symmetric Torus is capable of making electron temperature measurements via the double-filter technique; however, there has been a 15% systematic discrepancy between the SXR double-filter (SXR{sub DF}) temperature and Thomson scattering (TS) temperature. Here we discuss calibration of the Be filters used in the SXR{sub DF} measurement using empirical measurements of the transmission function versus energy at the BESSY II electron storage ring, electron microprobe analysis of filter contaminants, and measurement of the effective density. The calibration does not account for the TS and SXR{sub DF} discrepancy, and evidence frommore » experiments indicates that this discrepancy is due to physics missing from the SXR{sub DF} analysis rather than instrumentation effects.« less

Limitations on analysis of small particles with an electron probe: pollution studies

USGS Publications Warehouse

Heidel, R.H.; Desborough, G.A.

1975-01-01

Recent literature concerning the size and composition of airborne lead particles in automobile exhaust emissions determined by electron microprobe analysis reports 14 distinct lead compounds. Particle sizes reported were from 0.2 ??m to 2 ??m in the diameter. The determination of chemical formulae for compounds requires quantitative elemental data for individual particles. It was also assumed that the lead bearing particles analysed were solid (specifically non porous or non fluffy) compounds which occurred as discrete (non aggregate) particles. Intensity data obtained in the laboratory from the excited volume in a 1 ??m diameter sphere of solid lead chloride indicate insufficient precision and sensitivity to obtain chemical formulae as reported in the literature for exhaust emission products.

Ways to Improve the Quality of Die Steel 5KhNM

NASA Astrophysics Data System (ADS)

Efimov, S. V.; Malykhina, O. Yu; Pavlova, A. G.; Milyuts, V. G.; Tsukanov, V. V.; Vikharev, V. V.

2017-12-01

There was performed an analysis of influence of the deoxidation technology, hydrogen content and high concentration of titanium in steel 5KhNM (Rus. “5XHM”) on quality of die blanks, evaluated based on the results of the ultrasonic test. The fractographic examinations of fractures and the X-ray microprobe analysis of chemical composition of non-metallic inclusions were conducted, the evaluation of macro- and micro-structure of a die blank with high titanium content was performed. It is demonstrated that defects of dies from steel 5KhNM (Rus. “5XHM”) are cracks from merged flakes and micro-flakes; in most cases large concentrations of sulphides appeared to be hydrogen collectors for formation of flakes and micro-flakes.

Mineralogical characterization of rendering mortars from decorative details of a baroque building in Kozuchow (SW Poland)

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

Bartz, W., E-mail: wojciech.bartz@ing.uni.wroc.pl; Filar, T.

Optical microscopic observations, scanning electron microscopy and microprobe with energy dispersive X-ray analysis, X-ray diffraction and differential thermal/thermogravimetric analysis allowed detailed characterization of rendering mortars from decorative details (figures of Saints) of a baroque building in Kozuchow (Lubuskie Voivodship, Western Poland). Two separate coats of rendering mortars have been distinguished, differing in composition of their filler. The under coat mortar has filler composed of coarse-grained siliceous sand, whereas the finishing one has much finer grained filler, dominated by a mixture of charcoal and Fe-smelting slag, with minor amounts of quartz grains. Both mortars have air-hardening binder composed of gypsum andmore » micritic calcite, exhibiting microcrystalline structure.« 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

Different preparation methods and characterization of magnetic maghemite coated with chitosan

NASA Astrophysics Data System (ADS)

Hojnik Podrepšek, Gordana; Knez, Željko; Leitgeb, Maja

2013-06-01

The preparation of maghemite (γ-Fe2O3) micro- and nanoparticles coated with chitosan, used as carriers for immobilized enzymes, was investigated. γ-Fe2O3 nanoparticles were synthesized by coprecipitation of Fe2+ and Fe3+ ions in the presence of ammonium. They were coated with chitosan by the microemulsion process, suspension cross-linking technique, and covalent binding of chitosan on the γ-Fe2O3 surface. The methods distinguished the concentration of chitosan, concentration of acetic acid solution, concentration of a cross-linking agent, temperature of synthesis, pH of the medium, and time of synthesis. γ-Fe2O3 micro- and nanoparticles coated with chitosan prepared after three preparation methods were evaluated by scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectroscopy analysis, energy dispersive spectrometry, thermogravimetric analysis, differential scanning calorimetry analysis, vibrating sample magnetometry, dynamic light scattering, laser diffraction granulometry, and X-ray diffractometry. These positive attributes demonstrated that these magnetic micro- and nanoparticles coated with chitosan may be used as a promising carrier for further diverse biomedical applications.

The solubility and site preference of Fe3+ in Li7−3xFexLa3Zr2O12 garnets

PubMed Central

Rettenwander, D.; Geiger, C.A.; Tribus, M.; Tropper, P.; Wagner, R.; Tippelt, G.; Lottermoser, W.; Amthauer, G.

2015-01-01

A series of Fe3+-bearing Li7La3Zr2O12 (LLZO) garnets was synthesized using solid-state synthesis methods. The synthetic products were characterized compositionally using electron microprobe analysis and inductively coupled plasma optical emission spectroscopy (ICP-OES) and structurally using X-ray powder diffraction and 57Fe Mössbauer spectroscopy. A maximum of about 0.25 Fe3+ pfu could be incorporated in Li7−3xFexLa3Zr2O12 garnet solid solutions. At Fe3+ concentrations lower than about 0.16 pfu, both tetragonal and cubic garnets were obtained in the synthesis experiments. X-ray powder diffraction analysis showed only a garnet phase for syntheses with starting materials having intended Fe3+ contents lower than 0.52 Fe3+ pfu. Back-scattered electron images made with an electron microprobe also showed no phase other than garnet for these compositions. The lattice parameter, a0, for all solid-solution garnets is similar with a value of a0≈12.98 Å regardless of the amount of Fe3+. 57Fe Mössbauer spectroscopic measurements indicate the presence of poorly- or nano-crystalline FeLaO3 in syntheses with Fe3+ contents greater than 0.16 Fe3+ pfu. The composition of different phase pure Li7−3xFexLa3Zr2O12 garnets, as determined by electron microprobe (Fe, La, Zr) and ICP-OES (Li) measurements, give Li6.89Fe0.03La3.05Zr2.01O12, Li6.66Fe0.06La3.06Zr2.01O12, Li6.54Fe0.12La3.01Zr1.98O12, and Li6.19Fe0.19La3.02Zr2.04O12. The 57Fe Mössbauer spectrum of cubic Li6.54Fe0.12La3.01Zr1.98O12 garnet indicates that most Fe3+ occurs at the special crystallographic 24d position, which is the standard tetrahedrally coordinated site in garnet. Fe3+ in smaller amounts occurs at a general 96h site, which is only present for certain Li-oxide garnets, and in Li6.54Fe0.12La3.01Zr1.98O12 this Fe3+ has a distorted 4-fold coordination. PMID:26435549

PIXE analysis of caries related trace elements in tooth enamel

NASA Astrophysics Data System (ADS)

Annegarn, H. J.; Jodaikin, A.; Cleaton-Jones, P. E.; Sellschop, J. P. F.; Madiba, C. C. P.; Bibby, D.

1981-03-01

PIXE analysis has been applied to a set of twenty human teeth to determine trace element concentration in enamel from areas susceptible to dental caries (mesial and distal contact points) and in areas less susceptible to the disease (buccal surfaces), with the aim of determining the possible roles of trace elements in the curious process. The samples were caries-free anterior incisors extracted for periodontal reasons from subjects 10-30 years of age. Prior to extraction of the sample teeth, a detailed dental history and examination was carried out in each individual. PIXE analysis, using a 3 MeV proton beam of 1 mm diameter, allowed the determination of Ca, Mn, Fe, Cu, Zn, Sr and Pb above detection limits. As demonstrated in this work, the enhanced sensitivity of PIXE analysis over electron microprobe analysis, and the capability of localised surface analysis compared with the pooled samples required for neutron activation analysis, makes it a powerful and useful technique in dental analysis.

Solid state polymerization and crystallography of polyimide precursors. Ph.D. Thesis - Va. Univ.

NASA Technical Reports Server (NTRS)

Wakelyn, N. T.

1974-01-01

Although the production of crystallinity in a polymeric system has historically led to commerically useful properties, the polyimides, prized for their high temperature characteristics, as customarily synthesized by melt or solution casting, are amorphous. It is shown that polymide containing residual crystallinity can be synthesized by isothermal annealing of crystals of the salt of the diisopropyl ester of pyromellitic acid and phenylene diamine. The reaction is topochemical in that the geometry of the polymer product is dependent upon that of the crystalline precursor. Infrared spectroscopy reveals the presence of imide absorption in the polymer, while powder diffractometry suggests residual crystallinity. Single crystal X-ray analysis of the monomer yields a structure of chains of alternating acid and base suggesting that the monomer is amenable to polymerization with a minimum of geometrical disruption.

Leaching behavior and ESEM characterization of water-sensitive mudstone in southwestern Taiwan.

PubMed

Chen, Hung-Ta; Lin, Tzong-Tzeng; Chang, Juu-En

2003-05-01

This investigation attempts to understand the critical soluble salts in natural mudstone and the leaching, microstructural, and microchemical characteristics in soaked mudstone using scanning electron microscopy (SEM)/energy-dispersive X-ray analysis (EDAX), X-ray fluorescence spectrometry (XRF), X-ray diffractometry (XRD), conductivity measurement, ion chromatography (IC), and environmental scanning electron microscopy (ESEM)/EDAX techniques. Natural mudstone probably includes soluble salts such as Na2SO4, NaCl, NaCO3, and CaCO3. The dissolution of Na2SO4 controls water-sensitive mudstone very susceptible to slaking and dispersion. ESEM micrographs clearly show evidence of mudstone-slaking during soaking since the visible pores are filled with small aggregative masses. A calcium-bearing precipitate from the soaked mudstone is speculated to be attributable to the decomposition of the hydrated product of the fresh mudstone.

Analysis of NiAlTa precipitates in beta-NiAl + 2 at. pct Ta alloy

NASA Technical Reports Server (NTRS)

Pathare, V.; Michal, G. M.; Vedula, K.; Nathal, M. V.

1987-01-01

Results are reported from experiments performed to identify the precipitates, and their orientation in the matrix, in a beta-NiAl alloy containing 2 at. pct. Ta after undergoing creep test at 1300 K. Test specimens formed by extruding hot powders were compressed at 1300 K for about 50 hr at a strain rate averaging 6/1 million per sec. The specimens were then thinned and examined under an electron microscope and by X-ray diffractometry. An intermetallic NiAlTa compound with a hexagonal Cl4 structure appeared as second phase precipitates in the samples, exhibiting plate-like shapes and a habit plane close to (012). The prism planes of the hexagonal NiAlTa precipitates paralleled the closest packed planes in the cubic beta-NiAl matrix.

Alginate/cashew gum nanoparticles for essential oil encapsulation.

PubMed

de Oliveira, Erick F; Paula, Haroldo C B; de Paula, Regina C M

2014-01-01

Alginate/cashew gum nanoparticles were prepared via spray-drying, aiming at the development of a biopolymer blend for encapsulation of an essential oil. Nanoparticles were characterized regarding to their hydrodynamic volume, surface charge, Lippia sidoides essential oil content and release profile, in addition to being analyzed by infrared spectroscopy (FT-IR), thermal analysis (TGA/DSC) and X-ray diffractometry. Nanoparticles in solution were found to have averaged sizes in the range 223-399 nm, and zeta potential values ranging from -30 to -36 mV. Encapsulated oil levels varied from 1.9 to 4.4% with an encapsulation efficiency of up to 55%. The in vitro release profile showed that between 45 and 95% of oil was released within 30-50h. Kinetic studies revealed that release pattern follow a Korsmeyer-Peppas mechanism. Copyright © 2013 Elsevier B.V. All rights reserved.

Gold leaf counter electrodes for dye-sensitized solar cells

NASA Astrophysics Data System (ADS)

Shimada, Kazuhiro; Toyoda, Takeshi

2018-03-01

In this study, a gold leaf 100 nm thin film is used as the counter electrode in dye-sensitized solar cells. The traditional method of hammering gold foil to obtain a thin gold leaf, which requires only small amounts of gold, was employed. The gold leaf was then attached to the substrate using an adhesive to produce the gold electrode. The proposed approach for fabricating counter electrodes is demonstrated to be facile and cost-effective, as opposed to existing techniques. Compared with electrodes prepared with gold foil and sputtered gold, the gold leaf counter electrode demonstrates higher catalytic activity with a cobalt-complex electrolyte and higher cell efficiency. The origin of the improved performance was investigated by surface morphology examination (scanning electron microscopy), various electrochemical analyses (cyclic voltammetry, linear sweep voltammetry, and electrochemical impedance spectroscopy), and crystalline analysis (X-ray diffractometry).

Delaminating and restacking MgAl-layered double hydroxide monitored and characterized by a range of instrumental methods

NASA Astrophysics Data System (ADS)

Muráth, Szabolcs; Somosi, Zoltán; Tóth, Ildikó Y.; Tombácz, Etelka; Sipos, Pál; Pálinkó, István

2017-07-01

The delamination-restacking properties of MgAl-layered double hydroxide (MgAl-LDH) were studied in various solvents. The LDH samples were successfully delaminated in polar amides (formamide, N-methylformamide, N-methylacetamide). Usually, delamination was finalized by ultrasonic treatment. As rehydrating solutions, numerous Na-salts with single-, double- and triple-charged anions were used. Reconstruction was accomplished with anions of one or two negative charges, but triple-charged ones generally disrupted the rebuilding process, likely, because their salts with the metals of the LDH are very stable, and the thin layers can more readily transform to salts than the ordered materials. Samples and delamination-restacking processes were characterized by X-ray diffractometry (XRD), infrared spectroscopy (IR), dynamic light scattering (DLS), scanning electron microscopy (SEM) and energy-dispersive X-ray analysis (EDX).

Thermal behavior of potato starch and water-vaporization behavior of its paste controlled with amino acid and peptide-rich food materials.

PubMed

Sakauchi, Satoshi; Hattori, Makoto; Yoshida, Tadashi; Yagishita, Takahiro; Ito, Koichi; Akemitsu, Shin-Ichi; Takahashi, Koji

2010-03-01

The particular effect of 4 kinds of amino acid and peptide-rich food material (APRM) containing different charged amino acid contents on the gelatinization and retrogradation behavior of potato starch granules and on the water-vaporization behavior was analyzed by differential scanning calorimetry, rapid viscoanalysis, x-ray diffractometry, thermal gravimetry-differential thermal analysis, and pulsed NMR. APRM with a high-charged amino acid content produced unique gelatinization and retrogradation behavior in terms of an elevated gelatinization temperature, reduced viscosity, higher setback, and lower retrograded starch melting enthalpy. The recovered x-ray diffraction intensity decreased with increasing charged amino acid content. APRM with high-charged amino acid content could provide an improved paste having easy vaporization of external water in the swollen starch granules due to the reduced swelling.

Electrode erosion in steady-state electric propulsion engines

NASA Technical Reports Server (NTRS)

Pivirotto, Thomas J.; Deininger, William D.

1988-01-01

The anode and cathode of a 30 kW class arcjet engine were sectioned and analyzed. This arcjet was operated for a total time of 573 hr at power levels between 25 and 30 kW with ammonia at flow rates of 0.25 and 0.27 gm/s. The accumulated run time was sufficient to clearly establish erosion patterns and their causes. The type of electron emission from various parts of the cathode surface was made clear by scanning electron microscope analysis. A scanning electron microscope was used to study recrystallization on the hot anode surface. These electrodes were made of 2 percent thoriated tungsten and the surface thorium content and gradient perpendicular to the surfaces was determined by quantitative microprobe analysis. The results of this material analysis on the electrodes and recommendations for improving electrode operational life time are presented.

Watson: A new link in the IIE iron chain

NASA Technical Reports Server (NTRS)

Olsen, Edward; Davis, Andrew; Clarke, Roy S., Jr.; Schultz, Ludolf; Weber, Hartwig W.; Clayton, Robert; Mayeda, Toshiko; Jarosewich, Eugene; Sylvester, Paul; Grossman, Lawrence

1994-01-01

Watson, which was found in 1972 in South Australia, contains the largest single silicate rock mass seen in any known iron meteorite. A comprehensive study has been completed on this unusual meteorite: petrography, metallography, analyses of the silicate inclusion (whole rock chemical analysis, INAA, RNAA, noble gases, and oxygen isotope analysis) and mineral compositions (by electron microprobe and ion microprobe). The whole rock has a composition of an H-chondrite minus the normal H-group metal and troilite content. The oxygen isotope composition is that of the silicates in the IIE iron meteorites and lies along an oxygen isotope fractionation line with the H-group chondrites. Trace elements in the metal confirm Watson is a new IIE iron. Whole rock Watson silicate shows an enrichment in K and P (each approximately 2X H-chondrites). The silicate inclusion has a highly equilibrated igneous (peridotite-like) texture with olivine largely poikilitic within low-Ca pyroxene: olivine (Fa20), opx (Fs17Wo3), capx (Fs9Wo14)(with very fine exsolution lamellae), antiperthite feldspar (An1-3Or5) with less than 1 micron exsolution lamellae (An1-3Or greater than 40), shocked feldspar with altered stoichiometry, minor whitlockite (also a poorly characterized interstitial phosphate-rich phase) and chromite, and only traces of metal and troilite. The individual silicate minerals have normal chondritic REE patterns, but whitlockite has a remarkable REE pattern. It is very enriched in light REE (La is 720X C1, and Lu is 90X C1, as opposed to usual chonditic values of approximately 300X and 100-150X, respectively) with a negative Eu anomaly. The enrichment of whole rock K is expressed both in an unusually high mean modal Or content of the feldspar, Or13, and in the presence of antiperthite.

Development and application of laser microprobe techniques for oxygen isotope analysis of silicates, and, fluid/rock interaction during and after granulite-facies metamorphism, highland southwestern complex, Sri Lanka

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

Elsenheimer, D.W.

1992-01-01

The extent of fluid/rock interaction within the crust is a function of crustal depth, with large hydrothermal systems common in the brittle, hydrostatically pressured upper crust, but restricted fluid flow in the lithostatically pressured lower crust. To quantify this fluid/rock interaction, a Nd-YAG/CO[sub 2] laser microprobe system was constructed to analyze oxygen isotope ratios in silicates. Developed protocols produce high precision in [sigma][sup 18]O ([+-]0.2, 1[sigma]) and accuracy comparable to conventional extraction techniques on samples of feldspar and quartz as small as 0.3mg. Analysis of sub-millimeter domains in quartz and feldspar in granite from the Isle of Skye, Scotland, revealsmore » complex intragranular zonation. Contrasting heterogeneous and homogeneous [sigma][sup 18]O zonation patterns are revealed in samples <10m apart. These differences suggest fluid flow and isotopic exchange was highly heterogeneous. It has been proposed that granulite-facies metamorphism in the Highland Southwestern Complex (HSWC), Sri Lanka, resulted from the pervasive influx of CO[sub 2], with the marbles and calc-silicates within the HSWC a proposed fluid source. The petrologic and stable isotopic characteristic of HSWC marbles are inconsistent with extensive decarbonation. Wollastonite calc-silicates occur as deformed bands and as post-metamorphis veins with isotopic compositions that suggest vein fluids that are at least in part magmatic. Post-metamorphic magmatic activity is responsible for the formation of secondary disseminated graphite growth in the HSWC. This graphite has magmatic isotopic compositions and is associated with vein graphite and amphibolite-granulite facies transitions zones. Similar features in Kerela Khondalite Belt, South India, may suggest a common metamorphic history for the two terranes.« less

Microrisks for medical decision analysis.

PubMed

Howard, R A

1989-01-01

Many would agree on the need to inform patients about the risks of medical conditions or treatments and to consider those risks in making medical decisions. The question is how to describe the risks and how to balance them with other factors in arriving at a decision. In this article, we present the thesis that part of the answer lies in defining an appropriate scale for risks that are often quite small. We propose that a convenient unit in which to measure most medical risks is the microprobability, a probability of 1 in 1 million. When the risk consequence is death, we can define a micromort as one microprobability of death. Medical risks can be placed in perspective by noting that we live in a society where people face about 270 micromorts per year from interactions with motor vehicles. Continuing risks or hazards, such as are posed by following unhealthful practices or by the side-effects of drugs, can be described in the same micromort framework. If the consequence is not death, but some other serious consequence like blindness or amputation, the microrisk structure can be used to characterize the probability of disability. Once the risks are described in the microrisk form, they can be evaluated in terms of the patient's willingness-to-pay to avoid them. The suggested procedure is illustrated in the case of a woman facing a cranial arteriogram of a suspected arterio-venous malformation. Generic curves allow such analyses to be performed approximately in terms of the patient's sex, age, and economic situation. More detailed analyses can be performed if desired. Microrisk analysis is based on the proposition that precision in language permits the soundness of thought that produces clarity of action and peace of mind.

Nuclear Microprobe using Elastic Recoil Detection (ERD) for Hydrogen Profiling in High Temperature Protonic Conductors

NASA Technical Reports Server (NTRS)

Berger, Pascal; Sayir, Ali; Berger, Marie-Helene

2004-01-01

The interaction between hydrogen and various high temperature protonic conductors (HTPC) has not been clearly understood due to poor densification and unreacted secondary phases. the melt-processing technique is used in producing fully dense simple SrCe(0.9)Y (0.10) O(3-delta) and complex Sr3Ca(1+x)Nb(2+x)O(9-delta) perovskites that can not be achieved by solid-state sintering. the possibilities of ion beam analysis have been investigated to quantify hydrogen distribution in HTPC perovskites subjected to water heat treatment. Nuclear microprobe technique is based on the interactions of a focused ion beam of MeV light ions (H-1, H-2, He-3, He-4,.) with the sample to be analyzed to determine local elemental concentrations at the cubic micrometer scale, the elastic recoil detection analysis technique (ERDA) has been carried out using He-4(+) microbeams and detecting the resulting recoil protons. Mappings of longitudinal sections of water treated SrCeO3 and Sr(Ca(1/3)Nb(2/3))O3 perovskites have been achieved, the water treatment strongly alters the surface of simple SrCe(0.9)Y(0.10)O(3-delta) perovskite. From Rutherford Back Scattering measurements (RBS), both Ce depletion and surface re-deposition is evidenced. the ERDA investigations on water treated Sr3Ca(1+x)Nb(2+x)O(9-delta) perovskite did not exhibit any spatial difference for the hydrogen incorporation from the surface to the centre. the amount of hydrogen incorporation for Sr3Ca(1+x)Nb(2+x)O(9-delta) was low and required further development of two less conventional techniques, ERDA in forward geometry and forward elastic diffusion H-1(p,p) H-1 with coincidence detection.

Characteristic point algorithm in laser ektacytometry of red blood cells

NASA Astrophysics Data System (ADS)

Nikitin, S. Yu.; Ustinov, V. D.

2018-01-01

We consider the problem of measuring red blood cell deformability by laser diffractometry in shear flow (ektacytometry). A new equation is derived that relates the parameters of the diffraction pattern to the width of the erythrocyte deformability distribution. The numerical simulation method shows that this equation provides a higher accuracy of measurements in comparison with the analogous equation obtained by us earlier.

Single ion hit detection set-up for the Zagreb ion microprobe

NASA Astrophysics Data System (ADS)

Smith, R. W.; Karlušić, M.; Jakšić, M.

2012-04-01

Irradiation of materials by heavy ions accelerated in MV tandem accelerators may lead to the production of latent ion tracks in many insulators and semiconductors. If irradiation is performed in a high resolution microprobe facility, ion tracks can be ordered by submicrometer positioning precision. However, full control of the ion track positioning can only be achieved by a reliable ion hit detection system that should provide a trigger signal irrespectively of the type and thickness of the material being irradiated. The most useful process that can be utilised for this purpose is emission of secondary electrons from the sample surface that follows the ion impact. The status report of the set-up presented here is based on the use of a channel electron multiplier (CEM) detector mounted on an interchangable sample holder that is inserted into the chamber in a close geometry along with the sample to be irradiated. The set-up has been tested at the Zagreb ion microprobe for different ions and energies, as well as different geometrical arrangements. For energies of heavy ions below 1 MeV/amu, results show that efficient (100%) control of ion impact can be achieved only for ions heavier than silicon. The successful use of the set-up is demonstrated by production of ordered single ion tracks in a polycarbonate film and by monitoring fluence during ion microbeam patterning of Foturan glass.

PIXSIC: A Pixellated Beta-Microprobe for Kinetic Measurements of Radiotracers on Awake and Freely Moving Small Animals

NASA Astrophysics Data System (ADS)

Godart, J.; Weiss, P.; Chantepie, B.; Clemens, J. C.; Delpierre, P.; Dinkespiler, B.; Janvier, B.; Jevaud, M.; Karkar, S.; Lefebvre, F.; Mastrippolito, R.; Menouni, M.; Pain, F.; Pangaud, P.; Pinot, L.; Morel, C.; Laniece, P.

2010-06-01

We present a design study of PIXSIC, a new β+ radiosensitive microprobe implantable in rodent brain dedicated to in vivo and autonomous measurements of local time activity curves of beta radiotracers in a small (a few mm3) volume of brain tissue. This project follows the initial β microprobe previously developed at IMNC, which has been validated in several neurobiological experiments. This first prototype has been extensively used on anesthetized animals, but presents some critical limits for utilization on awake and freely moving animals. Consequently, we propose to develop a wireless setup that can be worn by an animal without constraints upon its movements. To that aim, we have chosen a Silicon-based detector, highly β sensitive, which allows for the development of a compact pixellated probe (typically 600 × 200 × 1000 μm3), read out with miniaturized wireless electronics. Using Monte-Carlo simulations, we show that high resistive Silicon pixels are appropriate for this purpose, assuming that the pixel dimensions are adapted to our specific signals. More precisely, a tradeoff has to be found between the sensitivity to β+ particles and to the 511 keV j background resulting from annihilations of β+ with electrons. We demonstrate that pixels with maximized surface and minimized thickness can lead to an optimization of their β+ sensitivity with a relative transparency to the annihilation background.

A view on elemental distribution alterations of coronary artery walls in atherogenesis

NASA Astrophysics Data System (ADS)

Pallon, J.; Homman, P.; Pinheiro, T.; Halpern, M. J.; Malmqvist, K.

1995-09-01

In this study, the Nuclear Microprobe technique was employed to investigate the elemental concentration alterations of minor and trace elements at the different cellular layers and structures of freeze-dried cryosections of human coronary arteries. Nuclear microprobe analyses enable to determine 7 elements, i.e., P, S, Cl, K, Ca, Fe and Zn in the artery walls. Furthermore, it was possible to identify early modifications of the artery due to the atherosclerosis progression that cannot be detected with specific staining or conventional histological methods. These modifications are shown to be related to abnormal Fe and Zn depositions in the surroundings of the elastic laminae. Later on, the calcifications of these regions occur, contributing to the elastic laminae damage and leading to the atheroma growing and maturation.

Transport of a high brightness proton beam through the Munich tandem accelerator

NASA Astrophysics Data System (ADS)

Moser, M.; Greubel, C.; Carli, W.; Peeper, K.; Reichart, P.; Urban, B.; Vallentin, T.; Dollinger, G.

2015-04-01

Basic requirement for ion microprobes with sub-μm beam focus is a high brightness beam to fill the small phase space usually accepted by the ion microprobe with enough ion current for the desired application. We performed beam transport simulations to optimize beam brightness transported through the Munich tandem accelerator. This was done under the constraint of a maximum ion current of 10 μA that is allowed to be injected due to radiation safety regulations and beam power constrains. The main influence of the stripper foil in conjunction with intrinsic astigmatism in the beam transport on beam brightness is discussed. The calculations show possibilities for brightness enhancement by using astigmatism corrections and asymmetric filling of the phase space volume in the x- and y-direction.

Pseudomorphic GeSiSn, SiSn and Ge layers in strained heterostructures

NASA Astrophysics Data System (ADS)

Timofeev, V. A.; Nikiforov, A. I.; Tuktamyshev, A. R.; Mashanov, V. I.; Loshkarev, I. D.; Bloshkin, A. A.; Gutakovskii, A. K.

2018-04-01

The GeSiSn, SiSn layer growth mechanisms on Si(100) were investigated and the kinetic diagrams of the morphological GeSiSn, SiSn film states in the temperature range of 150 °C-450 °C at the tin content from 0% to 35% were built. The phase diagram of the superstructural change on the surface of Sn grown on Si(100) in the annealing temperature range of 0 °C-850 °C was established. The specular beam oscillations were first obtained during the SiSn film growth from 150 °C to 300 °C at the Sn content up to 35%. The transmission electron microscopy and x-ray diffractometry data confirm the crystal perfection and the pseudomorphic GeSiSn, SiSn film state, and also the presence of smooth heterointerfaces between GeSiSn or SiSn and Si. The photoluminescence for the multilayer periodic GeSiSn/Si structures in the range of 0.6-0.8 eV was detected. The blue shift with the excitation power increase is observed suggesting the presence of a type II heterostructure. The creation of tensile strained Ge films, which are pseudomorphic to the underlying GeSn layer, is confirmed by the results of the formation and analysis of the reciprocal space map in the x-ray diffractometry. The tensile strain in the Ge films reached the value in the range of 0.86%-1.5%. The GeSn buffer layer growth in the Sn content range from 8% to 12% was studied. The band structure of heterosystems based on pseudomorphic GeSiSn, SiSn and Ge layers was calculated and the valence and conduction band subband position dependences on the Sn content were built. Based on the calculation, the Sn content range in the GeSiSn, SiSn, and GeSn layers, which corresponds to the direct bandgap GeSiSn, SiSn, and Ge material, was obtained.

Looking into individual coffee beans during the roasting process: direct micro-probe sampling on-line photo-ionisation mass spectrometric analysis of coffee roasting gases.

PubMed

Hertz-Schünemann, Romy; Streibel, Thorsten; Ehlert, Sven; Zimmermann, Ralf

2013-09-01

A micro-probe (μ-probe) gas sampling device for on-line analysis of gases evolving in confined, small objects by single-photon ionisation time-of-flight mass spectrometry (SPI-TOFMS) was developed. The technique is applied for the first time in a feasibility study to record the formation of volatile and flavour compounds during the roasting process within (inside) or in the direct vicinity (outside) of individual coffee beans. A real-time on-line analysis of evolving volatile and semi-volatile organic compounds (VOC and SVOC) as they are formed under the mild pyrolytic conditions of the roasting process was performed. The soft-ionisation mass spectra depict a molecular ion signature, which is well corresponding with the existing knowledge of coffee roasting and evolving compounds. Additionally, thereby it is possible to discriminate between Coffea arabica (Arabica) and Coffea canephora (Robusta). The recognized differences in the roasting gas profiles reflect the differences in the precursor composition of the coffee cultivars very well. Furthermore, a well-known set of marker compounds for Arabica and Robusta, namely the lipids kahweol and cafestol (detected in their dehydrated form at m/z 296 and m/z 298, respectively) were observed. If the variation in time of different compounds is observed, distinctly different evolution behaviours were detected. Here, phenol (m/z 94) and caffeine (m/z 194) are exemplary chosen, whereas phenol shows very sharp emission peaks, caffeine do not have this highly transient behaviour. Finally, the changes of the chemical signature as a function of the roasting time, the influence of sampling position (inside, outside) and cultivar (Arabica, Robusta) is investigated by multivariate statistics (PCA). In summary, this pilot study demonstrates the high potential of the measurement technique to enhance the fundamental knowledge of the formation processes of volatile and semi-volatile flavour compounds inside the individual coffee bean.

Layer dependence of the superconducting transition temperature of HgBa2Can-1 CunO2 n+2+ δ

NASA Astrophysics Data System (ADS)

Scott, B. A.; Suard, E. Y.; Tsuei, C. C.; Mitzi, D. B.; McGuire, T. R.; Chen, B.-H.; Walker, D.

1994-09-01

High-pressure methods have been used to synthesize multiphase compositions in the Hg12{ n-1} n homologous series. The phase assemblages were examined by optical, electron diffraction and X-ray diffraction techniques, and their stoichiometries verified by electron microprobe. Transport and magnetic susceptibility measurements were combined with the results of the phase analysis to establish superconducting transition temperatures for both as-prepared and O 2- or Ar-annealed materials. It was found that the transition temperature peaks at Tc = 134 K for n = 3 and then decreases abruptly for n>4, reaching Tc<90 K for n⪖7.

Microstructural study of the nickel-base alloy WAZ-20 using qualitative and quantitative electron optical techniques

NASA Technical Reports Server (NTRS)

Young, S. G.

1973-01-01

The NASA nickel-base alloy WAZ-20 was analyzed by advanced metallographic techniques to qualitatively and quantitatively characterize its phases and stability. The as-cast alloy contained primary gamma-prime, a coarse gamma-gamma prime eutectic, a gamma-fine gamma prime matrix, and MC carbides. A specimen aged at 870 C for 1000 hours contained these same constituents and a few widely scattered high W particles. No detrimental phases (such as sigma or mu) were observed. Scanning electron microscope, light metallography, and replica electron microscope methods are compared. The value of quantitative electron microprobe techniques such as spot and area analysis is demonstrated.

Northwest Africa 5298: A Basaltic Shergottite

NASA Technical Reports Server (NTRS)

Hui, Hejiu; Peslier, Anne; Lapen, Thomas J.; Brandon, Alan; Shafer, John

2009-01-01

NWA 5298 is a single 445 g meteorite found near Bir Gandouz, Morocco in March 2008 [1]. This rock has a brown exterior weathered surface instead of a fusion crust and the interior is composed of green mineral grains with interstitial dark patches containing small vesicles and shock melts [1]. This meteorite is classified as a basaltic shergottite [2]. A petrologic study of this Martian meteorite is being carried out with electron microprobe analysis and soon trace element analyses by laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). Oxygen fugacity is calculated from Fe-Ti oxides pairs in the sample. The data from this study constrains the petrogenesis of basaltic shergottites.

Segregation and inhomogeneities in photorefractive SBN fibers

NASA Astrophysics Data System (ADS)

Erdei, Sandor; Galambos, Ludwig; Tanaka, Isao; Hesselink, Lambertus; Ainger, Frank W.; Cross, Leslie E.; Feigelson, Robert S.

1996-10-01

Ce doped and undoped SrxBa1-xNb2O6 (SBN) fibers grown by the laser heated pedestal growth (LHPG) technique in Stanford University were investigated by 2D scanning electron microprobe analysis. The SBN fibers grown along c [001] or a [100] axes often show radially distributed optical inhomogeneities (core effects) of varying magnitude. Ba enrichment and Sr reduction were primarily detected in the core which can be qualitatively described by a complex-segregation effect. This defect structure as a complex-congruency related phenomenon modified by the composition-control mechanism of LHPG system. Its radial dependence of effective segregation coefficient is described by the modified Burton-Prim- Slichter equation.

Development of high temperature materials for solid propellant rocket nozzle applications. [tantalum carbides-tungsten fiber composites

NASA Technical Reports Server (NTRS)

Manning, C. R., Jr.; Honeycutt, L., III

1974-01-01

Evaluation of tantalum carbide-tungsten fiber composites has been completed as far as weight percent carbon additions and weight percent additions of tungsten fiber. Extensive studies were undertaken concerning Young's Modulus and fracture strength of this material. Also, in-depth analysis of the embrittling effects of the extra carbon additions on the tungsten fibers has been completed. The complete fabrication procedure for the tantalum carbide-tungsten fiber composites with extra carbon additions is given. Microprobe and metallographic studies showed the effect of extra carbon on the tungsten fibers, and evaluation of the thermal shock parameter fracture strength/Young's Modulus is included.

Phase relations in the system CuMoS

USGS Publications Warehouse

Dawei, H.; Chang, L.L.Y.; Knowles, C.R.

1990-01-01

Phase relations in the system CuMoS were studied in the temperature range 500-1000 ??C by using the conventional sealed, evacuated glass capsule technique. Reflected-light microscopy, X-ray powder diffraction and electron microprobe analysis were used for phase characterization. The chevrel-type phase, CuxMo3S4, is stable above 600??C, and forms equilibrium assemblages with the cubic Cu2S solid solution, copper, molybdenum, Mo2S3 and MoS2. Its solid solution ranges from Cu1.50-2.00Mo3S4 at 700??C to Cu1.22-2.00Mo3S4 at 1000 ??C. ?? 1990.

Textural variability of ordinary chondrite chondrules: Implications of their formation

NASA Technical Reports Server (NTRS)

Zinovieva, N. G.; Mitreikina, O. B.; Granovsky, L. B.

1994-01-01

Scanning electron microscopy (SEM) and microprobe examination of the Raguli H3-4, Saratov L3, and Fucbin L5-6 ordinary chondrites and the analysis of preexisted data on other meteorites have shown that the variety of textural types of chondrules depends on the chemical composition of the chondrules. The comparison of bulk-rock chemistries of the chondrules by major components demonstrates that they apparently fall, like basic-ultrabasic rock, into groups of dunitic and pyroxenitic composition. This separation is further validated by the character of zoning in chondrules of the intermediate, peridotitic type. The effect is vividly demonstrated by the 'chondrule-in-chondrule' structure.

STUDY OF URANIUM-ALUMINUM-IRON TERNARY CONSTITUTION DIAGRAM. Progress Report for the Period Ending March 31, 1963

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

Russell, R.B.

The determination of the U--Al-- Fe constitution diagram up to about 1000 ppm each of aluminum and iron is now being implemented by a determination of the U--Al and U-- Fe binary systems. The techniques to be used for this study include optical, electron and x-ray metallography, microprobe analysis, electrical resistance, and hothardness measurements. It is expected that a combination of techniques will give evidence of the amount of solid solubility of aluminum and iron in alpha uranium from 300 to 660 deg C, and in beta uranium at selected higher temperatures. (N.W.R.)

Scanning Electron Microscopy | Materials Science | NREL

Science.gov Websites

platform. The electron microprobe JEOL 8900L is the preference when quantitative composition of specimens , electroluminescence, lateral transport measurements, NFCL JEOL JXA-8900L Electron probe microanalysis Quantitative

Plasma properties and heating at the anode of a 1 kW arcjet using electrostatic probes

NASA Astrophysics Data System (ADS)

Tiliakos, Nicholas

A 1 kW hydrazine arcjet thruster has been modified for internal probing of the near-anode boundary layer with an array of fourteen electrostatic micro-probes. The main objectives of this experimental investigation were to: (1) obtain axial and azimuthal distributions of floating potential phisbf, anode sheath potential phisbs, probe current density at zero volts jsba, electron number density nsbes, electron temperature Tsbes, and anode heating due to electrons qsbe for arc currents Isbarc, between 7.8 and 10.6 A, propellant flow rates m = 40-60 mg/s, and specific energies, 18.8 MJ/kg ≤ P/m ≤ 27.4 MJ/kg; (2) probe the anode boundary layer using flush-mounted and cylindrical micro-probes; (3) verify azimuthal current symmetry; (4) understand what affects anode heating, a critical thruster lifetime issue; and (5) provide experimental data for validation of the Megli-Krier-Burton (MKB) model. All of the above objectives were met through the design, fabrication and implementation of fourteen electrostatic micro-probes, of sizes ranging from 0.170 mm to 0.43 mm in diameter. A technique for cleaning and implementing these probes was developed. Two configurations were used: flush-mounted planar probes and cylindrical probes extended 0.10-0.30 mm into the plasma flow. The main results of this investigation are: (1) electrostatic micro-probes can successfully be used in the harsh environment of an arcjet; (2) under all conditions tested the plasma is highly non-equilibrium in the near-anode region; (3) azimuthal current symmetry exists for most operating conditions; (4) the propellant flow rate affects the location of maximum anode sheath potential, current density, and anode heating more than the arc current; (5) the weighted anode sheath potential is always positive and varies from 8-17 V depending on thruster operating conditions; (6) the fraction of anode heating varies from 18-24% of the total input power over the range of specific energies tested; and (7) based on an energy loss factor of delta = 1200, reasonable correlation between the experimental data and the MKB model was found.

Electrodeposition of actinide compounds from an aqueous ammonium acetate matrix. Experimental development and optimization

DOE PAGES

Boll, Rose Ann; Matos, Milan; Torrico, Matthew N.

2015-03-27

Electrodeposition is a technique that is routinely employed in nuclear research for the preparation of thin solid films of actinide materials which can be used in accelerator beam bombardments, irradiation studies, or as radioactive sources. The present study investigates the deposition of both lanthanides and actinides from an aqueous ammonium acetate electrolyte matrix. Electrodepositions were performed primarily on stainless steel disks; with yield analysis evaluated using -spectroscopy. Experimental parameters were studied and modified in order to optimize the uniformity and adherence of the deposition while maximizing the yield. The initial development utilized samarium as the plating material, with and withoutmore » a radioactive tracer. As a result, surface characterization studies were performed by scanning electron microscopy, electron microprobe analysis, radiographic imaging, and x-ray diffraction.« less

Designing Ordered Molecular Arrays in Two and Three Dimensions

DTIC Science & Technology

1991-12-01

components often form 1:1 cocrystals (eq 1). These crystals are interesting for two R. R, H2. H H .R. N’.Hl H,.H𔃺 0 1 ’N ’N NH N N. NN No N .0’N N...and M. 35 Most seem to form 1:1 micro- cocrystals , most of which are not large enough for single- crystal diffractometry. Nonetheless, we have been able

Measuring skewness of red blood cell deformability distribution by laser ektacytometry

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

Nikitin, S Yu; Priezzhev, A V; Lugovtsov, A E

An algorithm is proposed for measuring the parameters of red blood cell deformability distribution based on laser diffractometry of red blood cells in shear flow (ektacytometry). The algorithm is tested on specially prepared samples of rat blood. In these experiments we succeeded in measuring the mean deformability, deformability variance and skewness of red blood cell deformability distribution with errors of 10%, 15% and 35%, respectively. (laser biophotonics)

Different decay patterns observed in a nineteenth-century building (Palma, Spain).

PubMed

Genestar, Catalina; Pons, Carmen; Cerro, José Carlos; Cerdà, Víctor

2014-01-01

The effects of atmospheric pollutants and climatic conditions were studied in a decayed column in the Seminary of Sant Pere. This nineteenth-century building is situated in the historic centre of Palma (Mallorca, Spain), less than 0.5 km from the sea. Samples were collected from the internal and external part of the crusts formed in the four sides of the column. The samples were analysed by means of thermal analysis, X-ray diffractometry, scanning electron microscopy, Fourier transform infrared spectroscopy and ion chromatography. Results show significant differences in the four sides of the column. A high degree of carbonate stone sulfation is observed in all of the samples analysed. A synergistic effect between atmospheric factors and micropollutants on the deterioration of stone is observed. A high uptake of atmospheric particulate matter is found in the external part of the black crusts.

Investigation of the Formation Process of Two Piracetam Cocrystals during Grinding

PubMed Central

Rehder, Sönke; Klukkert, Marten; Löbmann, Korbinian A. M.; Strachan, Clare J.; Sakmann, Albrecht; Gordon, Keith; Rades, Thomas; Leopold, Claudia S.

2011-01-01

Cocrystal formation rates during dry grinding and liquid-assisted grinding were investigated by X-ray powder diffractometry and Raman spectroscopy. Two polymorphic forms of piracetam were used to prepare known piracetam cocrystals as model substances, i.e., piracetam-citric acid and piracetam-tartaric acid cocrystals. Raman spectroscopy in combination with principal component analysis was used to visualize the cocrystal formation pathways. During dry grinding, cocrystal formation appeared to progress via an amorphous intermediate stage, which was more evident for the piracetam-citric acid than for the piracetam-tartaric acid cocrystal. It was shown that liquid-assisted grinding led to faster cocrystal formation than dry grinding, which may be explained by the higher transformation rate due to the presence of liquid. The cocrystal formation rate did not depend on the applied polymorphic form of the piracetam and no polymorphic cocrystals were obtained. PMID:24309304

Comparative analysis of strain fields in layers of step-graded metamorphic buffers of various designs

NASA Astrophysics Data System (ADS)

Aleshin, A. N.; Bugaev, A. S.; Ruban, O. A.; Tabachkova, N. Yu.; Shchetinin, I. V.

2017-10-01

Spatial distribution of residual elastic strain in the layers of two step-graded metamophic buffers of various designs, grown by molecular beam epitaxy from ternary InxAl1-xAs solutions on GaAs(001) substrates, is obtained using reciprocal space mapping by three-axis X-ray diffractometry and the linear theory of elasticity. The difference in the design of the buffers enabled the formation of a dislocation-free layer with different thickness in each of the heterostructures, which was the main basis of this study. It is shown that, in spite of the different design of graded metamorphic buffers, the nature of strain fields in them is the same, and the residual elastic strains in the final elements of both buffers adjusted for the effect of work hardening subject to the same phenomenological law, which describes the strain relief process in single-layer heterostructures.

Physicochemical analysis of Permian coprolites from Brazil

NASA Astrophysics Data System (ADS)

Rodrigues, M. I. C.; da Silva, J. H.; Santos, F. Eroni P.; Dentzien-Dias, P.; Cisneros, J. C.; de Menezes, A. S.; Freire, P. T. C.; Viana, B. C.

2018-01-01

In this paper we performed the study of two coprolites (fossilized feces) collected from the exposed levels of the Pedra de Fogo Formation, Parnaiba Sedimentary Basin, and Rio do Rasto Formation, Paraná Sedimentary Basin, both of the Palaeozoic era (Permian age). They were characterized using X-ray diffractometry, infrared, Raman and energy dispersive spectroscopy techniques in order to aid our understanding of the processes of fossilization and to discuss issues related to the feeding habits of the animals which generated those coprolites, probably cartilaginous fishes. The results obtained using a multitechnique approach showed that although these coprolites are from different geological formations, 3000 km away from each other, they show the same major crystalline phases and elemental composition. The main phases found were hydroxyapatite, silica, calcite and hematite, which lead to infer that those coprolites were formed under similar conditions and produced by a similar group of carnivore or omnivore fishes.

Tuning optical properties of CdTe films with nanocolumnar morphology grown using OAD for improving light absorption in thin-film solar cells

NASA Astrophysics Data System (ADS)

Daza, L. G.; Canché-Caballero, V.; Chan y Díaz, E.; Castro-Rodríguez, R.; Iribarren, A.

2017-11-01

CdTe films with transversal morphology in form of tilted nanocolumns were obtained by sublimation method using a rotating vapour source combined with the oblique angle deposition technique. The tilt angles of the nanocolumnar structures increases as the substrate inclination also increase. CdTe films exhibited cubic zinc blend lattice under compressive strain. Morphological and x-ray diffractometry analysis indicated that the nanocolumns are grains stacked in the nanocolumn preferential growth direction, except for the films with non-inclined substrate. We found an interesting dependence of band gap energy and the refractive index as functions of the microstrain distribution due to the nanocolumn tilt in the films from 0° to about 25°. These facts evidence the possibility of carried out film strain engineering for optimizing optoelectronics devices as we propose for the case of thin-film solar cells.

Solid state of CG-400549, a novel FabI inhibitor: characterization, dissolution, transformation.

PubMed

Kim, Bo-Yeon; Sohn, Young-Taek

2011-05-01

The polymorphic and pseudopolymorphic forms of CG-400549, a novel FabI inhibitor with potent in vivo activity were prepared and characterized by differential scanning calorimetry (DSC), powder X-ray diffractometry (PXRD) and thermogravimetric analysis (TG). Seven crystal forms of CG-400549, one anhydrate and six solvates, have been isolated by recrystallization and the DSC and PXRD patterns of the seven crystal forms of CG-400549 were different respectively. The dissolution patterns of these seven crystal forms of CG-400549 were studied and they showed significant differences in the dissolution rate. After storage of 1 month at 0% RH (silica gel, 20°C), 52% RH (saturated solution of Na(2)Cr(2)O(7)2H(2)O/20°C) and 95% RH (saturated solution of Na(2)HPO(4)/20°C), all crystal forms were not transformed.

A method of mounting multiple otoliths for beam-based microchemical analyses

USGS Publications Warehouse

Donohoe, C.J.; Zimmerman, C.E.

2010-01-01

Beam-based analytical methods are widely used to measure the concentrations of elements and isotopes in otoliths. These methods usually require that otoliths be individually mounted and prepared to properly expose the desired growth region to the analytical beam. Most analytical instruments, such as LA-ICPMS and ion and electron microprobes, have sample holders that will accept only one to six slides or mounts at a time. We describe a method of mounting otoliths that allows for easy transfer of many otoliths to a single mount after they have been prepared. Such an approach increases the number of otoliths that can be analyzed in a single session by reducing the need open the sample chamber to exchange slides-a particularly time consuming step on instruments that operate under vacuum. For ion and electron microprobes, the method also greatly reduces the number of slides that must be coated with an electrical conductor prior to analysis. In this method, a narrow strip of cover glass is first glued at one end to a standard microscope slide. The otolith is then mounted in thermoplastic resin on the opposite, free end of the strip. The otolith can then be ground and flipped, if needed, by reheating the mounting medium. After otolith preparation is complete, the cover glass is cut with a scribe to free the otolith and up to 20 small otoliths can be arranged on a single petrographic slide. ?? 2010 The Author(s).

Isotope Geochemistry of Possible Terrestrial Analogue for Martian Meteorite ALH84001

NASA Technical Reports Server (NTRS)

Mojzsis, Stephen J.

2000-01-01

We have studied the microdomain oxygen and carbon isotopic compositions by SIMS of complex carbonate rosettes from spinel therzolite xenoliths, hosted by nepheline basanite, from the island of Spitsbergen (Norway). The Quaternary volcanic rocks containing the xenoliths erupted into a high Arctic environment and through relatively thick continental crust containing carbonate rocks. We have attempted to constrain the sources of the carbonates in these rocks by combined O-18/O-16 and C-13/C-12 ratio measurements in 25 micron diameter spots of the carbonate and compare them to previous work based primarily on trace-element distributions. The origin of these carbonates can be interpreted in terms of either contamination by carbonate country rock during ascent of the xenoliths in the host basalt, or more probably by hydrothermal processes after emplacement. The isotopic composition of these carbonates from a combined delta.18O(sub SMOW) and delta.13C(sub PDB) standpoint precludes a primary origin of these minerals from the mantle. Here a description is given of the analysis procedure, standardization of the carbonates, major element compositions of the carbonates measured by electron microprobe, and their correlated C and O isotope compositions as measured by ion microprobe. Since these carbonate rosettes may represent a terrestrial analogue to the carbonate "globules" found in the martian meteorite ALH84001 interpretations for the origin of the features found in the Spitsbergen may be of interest in constraining the origin of these carbonate minerals on Mars.

A comparative study of modern and fossil cone scales and seeds of conifers: A geochemical approach

USGS Publications Warehouse

Artur, Stankiewicz B.; Mastalerz, Maria; Kruge, M.A.; Van Bergen, P. F.; Sadowska, A.

1997-01-01

Modern cone scales and seeds of Pinus strobus and Sequoia sempervirens, and their fossil (Upper Miocene, c. 6 Mar) counterparts Pinus leitzii and Sequoia langsdorfi have been studied using pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS), electron-microprobe and scanning electron microscopy. Microscopic observations revealed only minor microbial activity and high-quality structural preservation of the fossil material. The pyrolysates of both modern genera showed the presence of ligno-cellulose characteristic of conifers. However, the abundance of (alkylated)phenols and 1,2-benzenediols in modern S. sempervirens suggests the presence of non-hydrolysable tannins or abundant polyphenolic moieties not previously reported in modern conifers. The marked differences between the pyrolysis products of both modern genera are suggested to be of chemosystematic significance. The fossil samples also contained ligno-cellulose which exhibited only partial degradation, primarily of the carbohydrate constituents. Comparison between the fossil cone scale and seed pyrolysates indicated that the ligno-cellulose complex present in the seeds is chemically more resistant than that in the cone scales. Principal component analysis (PCA) of the pyrolysis data allowed for the determination of the discriminant functions used to assess the extent of degradation and the chemosystematic differences between both genera and between cone scales and seeds. Elemental composition (C, O, S), obtained using electron-microprobe, corroborated the pyrolysis results. Overall, the combination of chemical, microscopic and statistical methods allowed for a detailed characterization and chemosystematic interpretations of modern and fossil conifer cone scales and seeds.

Growth Structure and Properties of Gradient Nanocrystalline Coatings of the Ti-Al-Si-Cu-N System

NASA Astrophysics Data System (ADS)

Ovchinnikov, S. V.; Pinzhin, Yu. P.

2016-10-01

Methods of electron microprobe analysis, X-ray structure analysis and electron microscopy were used to study the element composition and features of the structure-phase, elastic stress state of nanocrystalline coatings of the Ti- Al- Si- Cu- N system with gradient of copper concentration across their thickness. The authors established the effects of element composition modification, non-monotonous behavior of the lattice constant of alloyed nitride and rise in the bending-torsion value of the crystalline lattice in individual nanocrystals to values of around 400 degrees/μm with increase in copper concentration, whereas the sizes of alloyed nitride crystals remained practically unchanged. Mechanical (hardness), adhesion and tribological properties of coatings were examined. Comparative analysis demonstrates higher values of adhesion characteristics in the case of gradient coatings of the Ti- Al- Si- Cu- N system than in the case of single-layer (with constant element concentration) analogues.

Nuclear analytical techniques in medicine

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

Cesareo, R.

1988-01-01

This book acquaints one with the fundamental principles and the instrumentation relevant to analytical technique based on atomic and nuclear physics, as well as present and future biomedical applications. Besides providing a theoretical description of the physical phenomena, a large part of the book is devoted to applications in the medical and biological field, particularly in hematology, forensic medicine and environmental science. This volume reviews methods such as the possibility of carrying out rapid multi-element analysis of trace elements on biomedical samples, in vitro and in vivo, by XRF-analysis; the ability of the PIXE-microprobe to analyze in detail and tomore » map trace elements in fragments of biomedical samples or inside the cells; the potentiality of in vivo nuclear activation analysis for diagnostic purposes. Finally, techniques are described such as radiation scattering (elastic and inelastic scattering) and attenuation measurements which will undoubtedly see great development in the immediate future.« less

XAP, a program for deconvolution and analysis of complex X-ray spectra

USGS Publications Warehouse

Quick, James E.; Haleby, Abdul Malik

1989-01-01

The X-ray analysis program (XAP) is a spectral-deconvolution program written in BASIC and specifically designed to analyze complex spectra produced by energy-dispersive X-ray analytical systems (EDS). XAP compensates for spectrometer drift, utilizes digital filtering to remove background from spectra, and solves for element abundances by least-squares, multiple-regression analysis. Rather than base analyses on only a few channels, broad spectral regions of a sample are reconstructed from standard reference spectra. The effects of this approach are (1) elimination of tedious spectrometer adjustments, (2) removal of background independent of sample composition, and (3) automatic correction for peak overlaps. Although the program was written specifically to operate a KEVEX 7000 X-ray fluorescence analytical system, it could be adapted (with minor modifications) to analyze spectra produced by scanning electron microscopes, electron microprobes, and probes, and X-ray defractometer patterns obtained from whole-rock powders.

Nuclear microanalysis of platinum and trace elements in cisplatin-resistant human ovarian adenocarcinoma cells

NASA Astrophysics Data System (ADS)

Moretto, P.; Ortega, R.; Llabador, Y.; Simonoff, M.; Bénard, J.; Moretto, Ph.

1995-09-01

Macro-and Micro-PIXE analysis were applied to study the mechanisms of cellular resistance to cisplatin, a chemotherapeutic agent, widely used nowadays for the treatment of ovarian cancer. Two cultured cell lines, a cisplatin-sensitive and a resistant one, were compared for their trace elements content and platinum accumulation following in vitro exposure to the drug. Bulk analysis revealed significant differences in copper and iron content between the two lines. Subsequent individual cell microanalysis permitted us to characterize the response of the different morphological cell types of the resistant line. This study showed that the metabolism of some trace metals in cisplatin-resistant cells could be affected but the exact relationship with the resistant phenotype remains to be determined. From a technical point of view, this experiment demonstrated that an accurate measurement of trace elements could be derived from nuclear microprobe analysis of individual cell.

A scanning proton microprobe study of stinging emergences from the leaf of the common stinging nettle urtica dioica l.

NASA Astrophysics Data System (ADS)

Hughes, N. P.; Perry, C. C.; Williams, R. J. P.; Watt, F.; Grime, G. W.

1988-03-01

Proton-induced X-ray emission (PIXE) combined with the Oxford scanning proton microprobe (SPM) was used to investigate the abundance and spatial distribution of inorganic elements in mineralising stinging emergences from the leaf of the Common Stinging Nettle, Urtica dioica L. Elemental maps and point analytical data were collected for emergences at two stages of maturity. In all emergences calcium and silicon were spatially organised and present at high concentration. The inorganic elements K, P, S and Mn were also spatially organised during mineralisation, but at maturity these elements were present only at background levels and then showed no specific localisation. The observed changes in the inorganic content of the emergences are obviously related to the mineralisation processes. The possible biochemical significance of the distribution of the elements is discussed.

Fast probe of local electronic states in nanostructures utilizing a single-lead quantum dot

PubMed Central

Otsuka, Tomohiro; Amaha, Shinichi; Nakajima, Takashi; Delbecq, Matthieu R.; Yoneda, Jun; Takeda, Kenta; Sugawara, Retsu; Allison, Giles; Ludwig, Arne; Wieck, Andreas D.; Tarucha, Seigo

2015-01-01

Transport measurements are powerful tools to probe electronic properties of solid-state materials. To access properties of local electronic states in nanostructures, such as local density of states, electronic distribution and so on, micro-probes utilizing artificial nanostructures have been invented to perform measurements in addition to those with conventional macroscopic electronic reservoirs. Here we demonstrate a new kind of micro-probe: a fast single-lead quantum dot probe, which utilizes a quantum dot coupled only to the target structure through a tunneling barrier and fast charge readout by RF reflectometry. The probe can directly access the local electronic states with wide bandwidth. The probe can also access more electronic states, not just those around the Fermi level, and the operations are robust against bias voltages and temperatures. PMID:26416582

Highly reproducible laser beam scanning device for an internal source laser desorption microprobe Fourier transform mass spectrometer

NASA Astrophysics Data System (ADS)

Scott, Jill R.; Tremblay, Paul L.

2002-03-01

Traditionally, mass spectrometry has relied on manipulating the sample target to provide scanning capabilities for laser desorption microprobes. This has been problematic for an internal source laser desorption Fourier transform mass spectrometer (LD-FTMS) because of the high magnetic field (7 Tesla) and geometric constraints of the superconducting magnet bore. To overcome these limitations, we have implemented a unique external laser scanning mechanism for an internal source LD-FTMS. This mechanism provides adjustable resolution enhancement so that the spatial resolution at the target is not limited to that of the stepper motors at the light source (˜5 μm/step). The spatial resolution is now limited by the practical optical diffraction limit of the final focusing lens. The scanning mechanism employs a virtual source that is wavelength independent up to the final focusing lens, which can be controlled remotely to account for focal length dependence on wavelength. A binary index provides an automatic alignment feature. The virtual source is located ˜9 ft from the sample; therefore, it is completely outside of the vacuum system and beyond the 50 G line of the fringing magnetic field. To eliminate reproducibility problems associated with vacuum pump vibrations, we have taken advantage of the magnetic field inherent to the FTMS to utilize Lenz's law for vibrational dampening. The LD-FTMS microprobe has exceptional reproducibility, which enables successive mapping sequences for depth-profiling studies.

Sample holder for X-ray diffractometry

DOEpatents

Hesch, Victor L.

1992-01-01

A sample holder for use with X-ray diffractometers with the capability to rotate the sample, as well as to adjust the position of the sample in the x, y, and z directions. Adjustment in the x direction is accomplished through loosening set screws, moving a platform, and retightening the set screws. Motion translators are used for adjustment in the y and z directions. An electric motor rotates the sample, and receives power from the diffractometer.

Single Crystal Diffractometry

NASA Astrophysics Data System (ADS)

Arndt, U. W.; Willis, B. T. M.

2009-06-01

Preface; Acknowledgements; Part I. Introduction; Part II. Diffraction Geometry; Part III. The Design of Diffractometers; Part IV. Detectors; Part V. Electronic Circuits; Part VI. The Production of the Primary Beam (X-rays); Part VII. The Production of the Primary Beam (Neutrons); Part VIII. The Background; Part IX. Systematic Errors in Measuring Relative Integrated Intensities; Part X. Procedure for Measuring Integrated Intensities; Part XI. Derivation and Accuracy of Structure Factors; Part XII. Computer Programs and On-line Control; Appendix; References; Index.

Craig L. Perkins, Ph.D. | NREL

Science.gov Websites

molecular beam epitaxy systems, two photoemission systems, a field-emission scanning Auger microprobe, a ;Molecular Anchors for Self-Assembled Monolayers on ZnO: A Direct Comparison of the Thiol and Phosphonic Acid

Modification of hectorite by organofunctionalization for use in removing U(VI) from aqueous media: thermodynamic approach.

PubMed

Guerra, Denis L; Airoldi, Claudio; Viana, Rúbia R

2010-02-01

A Hectorite sample (H) has been chemically modified with N-propyldiethylenetrimethoxysilane and bis[3-(triethoxysilyl)propyl]tetrasulfide. The resulting materials (H(3TPT) and H(NPTM)) have been characterized through elemental analysis, X-ray diffractometry, carbon nuclear magnetic resonance in the solid state, textural analysis, and thermogravimetric analysis. The adsorption experiments were performed under batch process with pH, ionic strength, contact time, and uranyl concentration as variables. The attached basic centers adsorbed uranyl cation to give maxima adsorption capacity of 5.55+/-0.21, 14.86+/-0.05, and 18.99+/-0.05 x 10(-3) mmol g(-1) for H, H(3TPT), and H(NPTM), respectively. From calorimetric determinations the quantitative thermal effects for UO(2)(2+)/center interactions gave exothermic enthalpy (Delta(int)H=-6.90 to -7.88 kJ mol(-1)), negative Gibbs free energy (Delta(int)G=-22.34 to -24.56 kJ mol(-1)), and positive entropy (Delta(int)S=51.80-56.00 JK(-1)mol(-1)). These thermodynamic data confirmed the energetically favorable condition of such interaction solid/liquid for all systems. Copyright 2009. Published by Elsevier Ltd.

DSC, X-ray and FTIR studies of a gemfibrozil/dimethyl-β-cyclodextrin inclusion complex produced by co-grinding.

PubMed

Aigner, Z; Berkesi, O; Farkas, G; Szabó-Révész, P

2012-01-05

The steps of formation of an inclusion complex produced by the co-grinding of gemfibrozil and dimethyl-β-cyclodextrin were investigated by differential scanning calorimetry (DSC), X-ray powder diffractometry (XRPD) and Fourier transform infrared (FTIR) spectroscopy with curve-fitting analysis. The endothermic peak at 59.25°C reflecting the melting of gemfibrozil progressively disappeared from the DSC curves of the products on increase of the duration of co-grinding. The crystallinity of the samples too gradually decreased, and after 35min of co-grinding the product was totally amorphous. Up to this co-grinding time, XRPD and FTIR investigations indicated a linear correlation between the cyclodextrin complexation and the co-grinding time. After co-grinding for 30min, the ratio of complex formation did not increase. These studies demonstrated that co-grinding is a suitable method for the complexation of gemfibrozil with dimethyl-β-cyclodextrin. XRPD analysis revealed the amorphous state of the gemfibrozil-dimethyl-β-cyclodextrin product. FTIR spectroscopy with curve-fitting analysis may be useful as a semiquantitative analytical method for discriminating the molecular and amorphous states of gemfibrozil. Copyright © 2011 Elsevier B.V. All rights reserved.

Archaeometallurgy in Messina: Iron Slug From A Dig at Blog P, Laboratory Analyses and Interpretation.

NASA Astrophysics Data System (ADS)

Caterina, Ingoglia; Maurizio, Triscari; Giuseppe, Sabatino

The archaeological site in Via La Farina, Block P, in Messina, is unique in many ways, due also to the high quantity of samples of iron slag. The slag was examined to identify the production centres of such materials, and, after characterization, was compared to similar material, exclusively for product typology, from different archaeological sites in the province of Messina, situated in the Peloritani Mountains (Messina city, S. Marco d'Alunzio, Milazzo, Francavilla di Sicilia, Novara di Sicilia as well as the archaeological site of Halaesa, near Tusa). Mineralogical characterization of the phases carried out by X-ray diffractometry (XRD) and Rietveld data elaboration, morphological study of slag findings and a semi-quantitative analysis by scanning electronic microscope (SEM+EDX) were performed. A chemical investigation was carried out by electron probe micro analysis (EPMA), to determine major element,. Minor and trace elements were determined by LA-ICP-MS. All the examined slag is related to iron metallurgy, and, in the case of Via La Farina, there is firm archaeological evidence pinpointing to smelting activity.

Effect of Heat Treatment Temperature on Chemical Compositions of Extracted Hydroxyapatite from Bovine Bone Ash

NASA Astrophysics Data System (ADS)

Younesi, M.; Javadpour, S.; Bahrololoom, M. E.

2011-11-01

This article presents the effect of heat treating temperature on chemical composition of hydroxyapatite (HA) that was produced by burning bovine bone, and then heat treating the obtained bone ash at different temperatures in range of 600-1100 °C in air. Bone ash and the resulting white powder from heat treating were characterized by Fourier transformed infrared spectroscopy (FT-IR) and x-ray diffractometry (XRD). The FT-IR spectra confirmed that heat treating of bone ash at temperature of 800 °C removed the total of organic substances. x-ray diffraction analysis showed that the white powder was HA and HA was the only crystalline phase indicated in heat treating product. x-ray fluorescence analyses revealed that calcium and phosphorous were the main elements and magnesium and sodium were minor impurities of produced powder at 800 °C. The results of the energy dispersive x-ray analysis showed that Ca/P ratio in produced HA varies in range of 1.46-2.01. The resulting material was found to be thermally stable up to 1100 °C.

Synthesis and Characterization of Cobalt Substituted Zinc Ferrite Nanoparticles by Microwave Combustion Method.

PubMed

Sundararajan, M; Kennedy, L John; Vijaya, J Judith

2015-09-01

Pure and cobalt doped zinc ferrites were prepared by microwave combustion method using L-arginine as a fuel. The prepared samples were characterized by various instrumental techniques such as X-ray powder diffractometry, high resolution scanning electron microscopy (HR-SEM), energy dispersive X-ray analysis, Fourier transformed infrared (FT-IR) spectroscopy, photoluminescence spectroscopy and UV-Visible diffuse reflectance spectroscopy. Vibrating sample magnetometry at room temperature was recorded to study the magnetic behavior of the samples. X-ray analysis confirmed the formation of zinc ferrites normal spinel-type structure with an average crystallite sizes in the range, 25.69 nm to 35.68 nm. The lattice parameters decreased as cobalt fraction was increased. The HR-SEM images showed nanoparticles are agglomerated. The estimated band gap energy value was found to decrease with an increase in cobalt content (1.87 to 1.62 eV). Broad visible emissions are observed in the photoluminescence spectra. A gradual increase in the coercivity and saturation magnetization (M(s)) were noted at relatively higher cobalt doping fractions.

Evaluation of phases in Pu-C-O and (U, Pu)-C-O systems by X-ray diffractometry and chemical analysis

NASA Astrophysics Data System (ADS)

Jain, G. C.; Ganguly, C.

1993-12-01

Preparation and characterisation of the carbides of uranium, plutonium and mixed uranium and plutonium form a part of advanced fuel development programs for fast breeder reactors. In the present study, the compositions of the phases of Pu-C-O and (U.Pu)-C-O systems have been determined by chemical analysis and lattice parameter measurement. The carbide samples have been prepared by vacuum carbothermic synthesis of tabletted oxide-graphite powder mixture. Dependence of stoichiometry of Pu 2C 3 phase on the oxygen content of Pu(C,O) phase in Pu(C,O) + Pu 2C 3 phase mixture has been evaluated. Stoichiometry and oxygen solubility of (U 0.3Pu 0.7)(C,O) phase in multiple phase mixture have been determined. Segregation of plutonium in (U,Pu) 2C 3 phase of (U,Pu)(C,O) + (U,Pu) 2C 3 phase mixture and its dependence on the oxygen content of (U,Pu)(C,O) phase have also been determined from the measurement of the lattice parameter of (U,Pu) 2C 3 phase.

Interdiffusion in the Ni/TD-NiCr and Cr/TD-NiCr systems

NASA Technical Reports Server (NTRS)

Pawar, A. V.; Tenney, D. R.

1974-01-01

The diffusion of Ni and Cr into TD-NiCr has been studied over the 900 to 1100 C temperature range. The diffusion couples were prepared by electroplating Cr and Ni on polished TD-NiCr wafers. Concentration profiles produced as a result of isothermal diffusion at 905, 1000, and 1100 C were determined by electron microprobe analysis. The Boltzmann-Matano analysis was used to determine concentration-dependent diffusion coefficients which were found to compare favorably with previously reported values. These data suggest that 2 vol % ThO2 distribution has no appreciable effect on the rates of diffusion in TD-NiCr with a large grain size. This supports the view that an inert dispersoid in an alloy matrix will not in itself lead to enhanced diffusion unless a short-circuit diffusion structure is stabilized.

Accelerator-based analytical technique in the evaluation of some Nigeria’s natural minerals: Fluorite, tourmaline and topaz

NASA Astrophysics Data System (ADS)

Olabanji, S. O.; Ige, O. A.; Mazzoli, C.; Ceccato, D.; Akintunde, J. A.; De Poli, M.; Moschini, G.

2005-10-01

For the first time, the complementary accelerator-based analytical technique of PIXE and electron microprobe analysis (EMPA) were employed for the characterization of some Nigeria's natural minerals namely fluorite, tourmaline and topaz. These minerals occur in different areas in Nigeria. The minerals are mainly used as gemstones and for other scientific and technological applications and therefore are very important. There is need to characterize them to know the quality of these gemstones and update the geochemical data on them geared towards useful applications. PIXE analysis was carried out using the 1.8 MeV collimated proton beam from the 2.5 MV AN 2000 Van de Graaff accelerator at INFN, LNL, Legnaro, Padova, Italy. The novel results which show many elements at different concentrations in these minerals are presented and discussed.

Preliminary study on the mode of occurrence of arsenic in high arsenic coals from southwest Guizhou Province

USGS Publications Warehouse

Ding, Z.; Zheng, B.; Zhang, Jiahua; Belkin, H.E.; Finkelman, R.B.; Zhao, F.; Zhou, D.; Zhou, Y.; Chen, C.

1999-01-01

Coal samples from high arsenic coal areas have been analyzed by electron microprobe analyzer (EMPA), scanning electron microscopy with an energy dispersive X-ray analyzer (SEM-EDX), X-ray diffraction analysis (XRD), low temperature ashing (LTA), transmission electron microscopy (TEM), X-ray absorption fine structure (XAFS), instrument neutron activation analysis (INAA) and wet chemical analysis. Although some As-bearing minerals such as pyrite, arsenopyrite, realgar (?), As-bearing sulfate, and As-bearing clays are found in the high arsenic coals, their contents do not account for the abundance of arsenic in the some coals. Analysis of the coal indicates that arsenic exists mainly in the form of As5+ and As3+, combined with compounds in the organic matrix. The occurrence of such exceptionally high arsenic contents in coal and the fact that the arsenic is dominantly organically associated are unique observations. The modes of occurrence of arsenic in high As-coals are discussed.

Reverse engineering the physical chemistry of making Egyptian faience through compositional analysis of the cementation process

NASA Astrophysics Data System (ADS)

Pourattar, Parisa

The cementation process of making Egyptian faience, reported by Hans Wulff from a workshop in Qom, Iran, has not been easy to replicate and various views have been set forth to understand the transport of materials from the glazing powder to the surfaces of the crushed quartz beads. Replications of the process fired to 950° C and under-fired to 850° C were characterized by electron beam microprobe analysis (EPMA), petrographic thin section analysis, and scanning electron microscopy with energy dispersive x-ray analysis (SEM-EDS). Chemical variations were modeled using thermal data, phase diagrams, and copper vaporization experiments. These replications were compared to 52 examples from various collections, including 20th century ethnographic collections of beads, glazing powder and plant ash, 12th century CE beads and glazing powder from Fustat (Old Cairo), Egypt, and to an earlier example from Abydos, Egypt in the New Kingdom and to an ash example from the Smithsonian Institution National Museum of Natural History.

Petrology and Geochemistry of the NWA 3368 Eucrite

NASA Astrophysics Data System (ADS)

Gardner, K. G.; Lauretta, D. S.; Hill, D. H.; Goreva, J. S.; Domanik, K. J.; Franchi, I. A.; Drake, M. J.

2006-03-01

We report the petrology and geochemistry of NWA 3368, a new non-cumulate, monomict eucrite breccia with a variety of clast sizes and a pink-tinted matrix. Analytical techniques include electron microprobe, INAA, and ICP-MS.

Inter- and intra-group compositional variations in Apollo 15 pyroclastic green glass - An electron- and ion-microprobe study

NASA Technical Reports Server (NTRS)

Galbreath, K. C.; Shearer, C. K.; Papike, J. J.; Shimizu, N.

1990-01-01

Results are presented on major- and trace-element abundance analyses of Apollo 15 pyroclastic green glasses from groups A, B, C, D, and E, carried out using electron- and ion-microprobe techniques. The diagrams depicting Sr, Zr, Ba, and Nd vs Co variations indicate the presence of a high-Co trend in groups A and D and a low-Co trend in groups B and C. Group-E glasses were found to be significantly enriched in Sr, relative to the other four glass groups. Chemical data of this study were integrated with previous data to evaluate various magmatic processes that have been proposed in the past to explain chemical variations in the lunar green glass. Results of calculations using a source mixing model suggest that the Apollo 15 green glasses represent multiple eruptive events from three chemically distinct but compositionally variable source regions.

A petrologic and ion microprobe study of a Vigarano Type B refractory inclusion - Evolution by multiple stages of alteration and melting

NASA Technical Reports Server (NTRS)

Macpherson, Glenn J.; Davis, Andrew M.

1993-01-01

A Type B Ca-, Al-rich 6-m-diam inclusion (CAI) found in the Vigarano C3V chondrite was inspected using optical and scanning electron microscopies and ion microprobe analyses. It was found that the primary constituents of the CAI inclusion are (in percent), melilite (52), fassaite, (20), anorthite (18), spinel (10), and trace Fe-Ni metal. It is noted that, while many of the properties of the inclusion indicate solidification from a melt droplet, the Al-26/Mg-26 isotopic systematics and some textural relationships are incompatible with single-stage closed system crystallization of a homogeneous molten droplet, indicating that the history of this inclusion must have been more complex than melt solidification alone. Moreover, there was unusually high content of Na in melilite, suggesting that the droplet did not form by melting of pristine high-temperature nebular condensates.

Nuclear microprobe investigation of the penetration of ultrafine zinc oxide into intact and tape-stripped human skin

NASA Astrophysics Data System (ADS)

Szikszai, Z.; Kertész, Zs.; Bodnár, E.; Major, I.; Borbíró, I.; Kiss, Á. Z.; Hunyadi, J.

2010-06-01

Ultrafine metal oxides, such as titanium dioxide and zinc oxide are widely used in cosmetic and health products like sunscreens. These oxides are potent UV filters and the small particle size makes the product more transparent compared to formulations containing coarser particles. In the present work the penetration of ultrafine zinc oxide into intact and tape-stripped human skin was investigated using nuclear microprobe techniques, such as proton induced X-ray spectroscopy and scanning transmission ion microscopy. Our results indicate that the penetration of ultrafine zinc oxide, in a hydrophobic basis gel with 48 h application time, is limited to the stratum corneum layer of the intact skin. Removing the stratum corneum partially or entirely by tape-stripping did not cause the penetration of the particles into the deeper dermal layers; the zinc particles remained on the surface of the skin.

Laser microprobe and resonant laser ablation for depth profile measurements of hydrogen isotope atoms contained in graphite.

PubMed

Yorozu, M; Yanagida, T; Nakajyo, T; Okada, Y; Endo, A

2001-04-20

We measured the depth profile of hydrogen atoms in graphite by laser microprobing combined with resonant laser ablation. Deuterium-implanted graphite was employed for the measurements. The sample was ablated by a tunable laser with a wavelength corresponding to the resonant wavelength of 1S-2S of deuterium with two-photon excitation. The ablated deuterium was ionized by a 2 + 1 resonant ionization process. The ions were analyzed by a time-of-flight mass spectrometer. The deuterium ions were detected clearly with the resonant ablation. The detection limit was estimated to be less than 10(16) atoms/cm(3) in our experiments. We determined the depth profile by considering the etching profile and the etching rate. The depth profile agreed well with Monte Carlo simulations to within a precision of 23 mum for the center position and 4-mum precision for distributions for three different implantation depths.

Electron microprobe analyses of Ca, S, Mg and P distribution in incisors of Spacelab-3 rats

NASA Technical Reports Server (NTRS)

Rosenberg, G. D.; Simmons, D. J.

1985-01-01

The distribution of Ca, S, Mg and P was mapped within the incisors of Spacelab-3 rats using an electron microprobe. The data indicate that Flight rats maintained in orbit for 7 days have significantly higher Ca/Mg ratios in dentin due to both higher Ca and lower Mg content than in dentin of ground-based Controls. There is no statistical difference in distribution of either P or S within Fligth animals and Controls, but there is clear indication that, for P at least, the reason is the greater variability of the Control data. These results are consistent with those obtained on a previous NASA/COSMOS flight of 18.5 days duration, although they are not pronounced. The results further suggest that continuously growing rat incisors provide useful records of the effects of weightlessness on Ca metabolism.

A high excitation magnetic quadrupole lens quadruplet incorporating a single octupole lens for a low spherical aberration probe forming lens system

NASA Astrophysics Data System (ADS)

Dou, Yanxin; Jamieson, David N.; Liu, Jianli; Li, Liyi

2018-03-01

This paper describes the design of a new probe forming lens system consisting of a high excitation magnetic quadrupole lens quadruplet that incorporates a single magnetic octupole lens. This system achieves both a high demagnification and a low spherical aberration compared to conventional high excitation systems and is intended for deployment for the Harbin 300 MeV proton microprobe for applications in space science and ion beam therapy. This relative simplicity of the ion optical design to include a single octupole lens minimizes the risks associated with the constructional and operational precision usually needed for the probe forming lens system and this system could also be deployed in microprobe systems that operate with less magnetically rigid ions. The design of the new system is validated with reference to two independent ion optical computer codes.

Secondary ion collection and transport system for ion microprobe

DOEpatents

Ward, James W.; Schlanger, Herbert; McNulty, Jr., Hugh; Parker, Norman W.

1985-01-01

A secondary ion collection and transport system, for use with an ion microprobe, which is very compact and occupies only a small working distance, thereby enabling the primary ion beam to have a short focal length and high resolution. Ions sputtered from the target surface by the primary beam's impact are collected between two arcuate members having radii of curvature and applied voltages that cause only ions within a specified energy band to be collected. The collected ions are accelerated and focused in a transport section consisting of a plurality of spaced conductive members which are coaxial with and distributed along the desired ion path. Relatively high voltages are applied to alternate transport sections to produce accelerating electric fields sufficient to transport the ions through the section to an ion mass analyzer, while lower voltages are applied to the other transport sections to focus the ions and bring their velocity to a level compatible with the analyzing apparatus.

KSC-98pc1625

NASA Image and Video Library

1998-11-10

KENNEDY SPACE CENTER, FLA. -- In the Spacecraft Assembly and Encapsulation Facility -2 (SAEF-2), the Mars Polar Lander is prepared to receive a number of microprobes being added to the spacecraft. Scheduled to be launched on Jan. 3, 1999, the solar-powered spacecraft is designed to touch down on the Martian surface near the northern-most boundary of the south pole in order to study the water cycle there. The lander also will help scientists learn more about climate change and current resources on Mars, studying such things as frost, dust, water vapor and condensates in the Martian atmosphere. The Mars microprobes will complement the climate-related scientific focus of the lander by demonstrating an advanced, rugged microlaser system for detecting subsurface water. Such data on polar subsurface water, in the form of ice, should help put limits on scientific projections for the global abundance of water on Mars

Hg diffusion in books of XVIII and XIX centuries by synchrotron microprobe

NASA Astrophysics Data System (ADS)

Pessanha, S.; Carvalho, M. L.; Manso, M.; Guilherme, A.; Marques, A. F.; Perez, C. A.

2009-08-01

The pigment vermilion (HgS) was used to color the fore edge, tail and head of books. Dissemination and quantification of Hg present in the ink used to color books from XVIII and XIX centuries are reported. Mercury is a very toxic element for the human body, therefore it is extremely important to know whether Hg tends to disseminate throughout the paper or stays confined to the borders of the books with less danger for readers. Synchrotron X-ray microprobe was used to evaluate Hg dissemination from the border to the centre of the paper sheet. The diffusion pattern of Hg was compared with the results obtained by a portable X-ray fluorescence spectrometer and mean quantitative calculations were obtained by a stationary X-ray fluorescence system with triaxial geometry. The results showed high concentrations of Hg in the external regions, but no diffusion was observed for the inner parts of the paper.

Elemental maps of Amoeba proteus by a scanning proton microprobe

NASA Astrophysics Data System (ADS)

Li, Minqian; Zhu, Jingde; Zhu, Jieqing; Zhou, Zheng; Huang, Zeqi; Zhou, Weiying; Cholewa, M.; Legge, G. J. F.

1991-03-01

Elemental maps for P, S, Cl, K, Ca and Zn of individual Amoeba proteus were obtained with the Melbourne scanning proton microprobe. The emphasis was put on the relationship of both distribution and concentration of Zn within the cell and the growth inhibitory effect of higher Zn concentrations in the culture medium. At a concentration of 0.04 mmol ZnCl 2, Amoeba growth was inhibited. But at a concentration of 0.0016 mmol, the Amoeba grew as well as a control grown without addition of Zn. We found that in the former (0.04 mmol) Zn concentrated three times more than in the latter (0.0016 mmol), and also that Zn was enriched much more in the nucleus and endoplasm (five to six times) than in other parts of the cell (two times). Future work along these lines may provide insight into the mechanism by which Zn affects the growth of Amoeba proteus and other cells.

In-situ characterization of nanoparticle beams focused with an aerodynamic lens by Laser-Induced Breakdown Detection

PubMed Central

Barreda, F.-A.; Nicolas, C.; Sirven, J.-B.; Ouf, F.-X.; Lacour, J.-L.; Robert, E.; Benkoula, S.; Yon, J.; Miron, C.; Sublemontier, O.

2015-01-01

The Laser-Induced Breakdown Detection technique (LIBD) was adapted to achieve fast in-situ characterization of nanoparticle beams focused under vacuum by an aerodynamic lens. The method employs a tightly focused, 21 μm, scanning laser microprobe which generates a local plasma induced by the laser interaction with a single particle. A counting mode optical detection allows the achievement of 2D mappings of the nanoparticle beams with a reduced analysis time thanks to the use of a high repetition rate infrared pulsed laser. As an example, the results obtained with Tryptophan nanoparticles are presented and the advantages of this method over existing ones are discussed. PMID:26498694

Corrosion phenomena in electron, proton and synchrotron X-ray microprobe analysis of Roman glass from Qumran, Jordan

NASA Astrophysics Data System (ADS)

Janssens, K.; Aerts, A.; Vincze, L.; Adams, F.; Yang, C.; Utui, R.; Malmqvist, K.; Jones, K. W.; Radtke, M.; Garbe, S.; Lechtenberg, F.; Knöchel, A.; Wouters, H.

1996-04-01

A series of 89 glass fragments of Roman glass are studied using electron, proton and synchrotron radiation induced X-ray emission from microscopic areas on the sample surface. The glass originates from Qumran, Jordan and was buried for 1900 years. The weathering layers that result from the extended contact with ground water have been studied, next to the trace composition of the original glass of these pieces. The latter information indicates that at Qumran, large quantities of glass objects were being used in Ancient times. Cross-sectional profiles of the glass show a complex migration behaviour of various groups of major and trace elements.

Evidence for extreme Ti-50 enrichments in primitive meteorites

NASA Technical Reports Server (NTRS)

Fahey, A.; Mckeegan, K. D.; Zinner, E.; Goswami, J. N.

1985-01-01

The results of the first high mass resolution ion microprobe study of Ti isotopic compositions in individual refractory grains from primitive carbonaceous meteorites are reported. One hibonite from the Murray carbonaceous chondrite has a 10 percent excess of Ti-50, 25 times higher than the maximum value previously reported for bulk samples of refractory inclusions from carbonaceous chondrites. The variation of the Ti compositions between different hibonite grains, and among pyroxenes from a single Allende refractory inclusion, indicates isotopic inhomogeneities over small scale lengths in the solar nebula and emphasizes the importance of the analysis of small individual phases. This heterogeneity makes it unlikely that the isotopic anomalies were carried into the solar system in the gas phase.

Analyses of amphibole asbestiform fibers in municipal water supplies

PubMed Central

Nicholson, William J.

1974-01-01

Details are given of the techniques used in the analysis of asbestiform fibers in the water systems of Duluth, Minnesota and other cities. Photographic electron diffraction and electron microprobe analyses indicated that the concentration of verified amphibole mineral fibers ranged from 20 × 106 to 75 × 106 fibers/l. Approximately 50–60% of the fibers were in the cummingtonite-grunerite series and 20% were in the actinolite-tremolite series. About 5% were chemically identical with amosite. A wide variety of analytical techniques must be employed for unique identification of the mineral species present in water systems. ImagesFIGURE 1.FIGURE 2.FIGURE 3.FIGURE 4.FIGURE 5.FIGURE 6. PMID:4470931

Ion beam microanalysis of human hair follicles

NASA Astrophysics Data System (ADS)

Kertész, Zs.; Szikszai, Z.; Pelicon, P.; Simčič, J.; Telek, A.; Bíró, T.

2007-07-01

Hair follicle is an appendage organ of the skin which is of importance to the survival of mammals and still maintains significance for the human race - not just biologically, but also through cosmetic and commercial considerations. However data on composition of hair follicles are scarce and mostly limited to the hair shaft. In this study we provide detailed information on the elemental distribution in human hair follicles in different growth phases (anagen and catagen) using a scanning proton microprobe. The analysis of skin samples obtained from human adults undergoing plastic surgery and of organ-cultured human hair follicles may yield a new insight into the function, development and cyclic activity of the hair follicle.

Mineralogy and Microstructures of Shock-Induced Melt Veins in Chondrites

NASA Technical Reports Server (NTRS)

Sharp, Thomas G.

2000-01-01

The applicability of phase equilibrium data to the interpretation of shock-induced melt veins can only be tested by a detailed study of melt- vein mineralogy to see how high-pressure assemblages vary as a function of shock conditions inferred from other indicators. We have used transmission electron microscopy (TEM), analytical electron microscopy (AEM), scanning electron microscopy (SEM), electron microprobe analysis (EMA) and optical petrography to characterize the mineralogy, microstructures, and compositions of melt veins and associated high-pressure minerals in shocked chondrites and SNC meteorites. In the processes, we have gained a better understanding of what melt veining can tell us about shock conditions and we have discovered new mineral phases in chondritic and SNC meteorites.

Grains of Nonferrous and Noble Metals in Iron-Manganese Formations and Igneous Rocks of Submarine Elevations of the Sea of Japan

NASA Astrophysics Data System (ADS)

Kolesnik, O. N.; Astakhova, N. V.

2018-01-01

Iron-manganese formations and igneous rocks of submarine elevations in the Sea of Japan contain overlapping mineral phases (grains) with quite identical morphology, localization, and chemical composition. Most of the grains conform to oxides, intermetallic compounds, native elements, sulfides, and sulfates in terms of the set of nonferrous, noble, and certain other metals (Cu, Zn, Sn, Pb, Ni, Mo, Ag, Pd, and Pt). The main conclusion that postvolcanic hydrothermal fluids are the key sources of metals is based upon a comparison of the data of electron microprobe analysis of iron-manganese formations and igneous rocks dredged at the same submarine elevations in the Sea of Japan.

Composition, structure, and properties of iron-rich nontronites of different origins

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

Palchik, N. A., E-mail: nadezhda@igm.nsc.ru; Grigorieva, T. N.; Moroz, T. N.

2013-03-15

The composition, structure, and properties of smectites of different origins have been studied by X-ray diffraction, IR spectroscopy, scanning electron microscopy, and microprobe analysis. The results showed that nontronites of different origins differ in composition, properties, morphology, and IR spectroscopic characteristics. Depending on the degree of structural order and the negative charge of iron-silicate layers in nontronites, the shift of the 001 reflection to smaller angles as a result of impregnation with ethylene glycol (this shift is characteristic of the smectite group) occurs differently. The calculated values of the parameter b (from 9.11 to 9.14A) are valid for the extrememore » terms of dioctahedral smectite representatives: nontronites.« less

Measurement of in situ sulfur isotopes by laser ablation multi-collector ICPMS: opening Pandora’s Box

USGS Publications Warehouse

Ridley, William I.; Pribil, Michael; Koenig, Alan E.; Slack, John F.

2015-01-01

Laser ablation multi-collector ICPMS is a modern tool for in situ measurement of S isotopes. Advantages of the technique are speed of analysis and relatively minor matrix effects combined with spatial resolution sufficient for many applications. The main disadvantage is a more destructive sampling mechanism relative to the ion microprobe technique. Recent advances in instrumentation allow precise measurement with spatial resolutions down to 25 microns. We describe specific examples from economic geology where increased spatial resolution has greatly expanded insights into the sources and evolution of fluids that cause mineralization and illuminated genetic relations between individual deposits in single mineral districts.

Studies of Halogen Bonding Using High-Pressure Diffractometry

DTIC Science & Technology

2007-11-08

mixed at room temperature. The 1:1 cocrystal was melted by heating it to and in the liquid form loaded to a DAC. Single-crystal of each compound or...upper edge. Figure 6. Isochoric growth of the 1,2-diiodoperfluoroethane:1,4-dioxane 1:1 cocrystal : (a) the melting process of the polycrystal...impurities in the mixture, which condensed at high pressure and grouped between the cocrystal upper face (001) and the upper culet. Figure 7. Isochoric

Migration and rearing histories of chinook salmon (Oncorhynchus tshawytscha) determined by ion microprobe Sr isotope and Sr/Ca transects of otoliths

USGS Publications Warehouse

Bacon, C.R.; Weber, P.K.; Larsen, K.A.; Reisenbichler, R.; Fitzpatrick, J.A.; Wooden, J.L.

2004-01-01

Strontium isotope and Sr/Ca ratios measured in situ by ion microprobe along radial transects of otoliths of juvenile chinook salmon (Oncorhynchus tshawytscha) vary between watersheds with contrasting geology. Otoliths from ocean-type chinook from Skagit River estuary, Washington, had prehatch regions with 87Sr/86Sr ratios of ???0.709, suggesting a maternally inherited marine signature, extensive fresh water growth zones with 87Sr/86Sr ratios similar to those of the Skagit River at ???0.705, and marine-like 87Sr/86Sr ratios near their edges. Otoliths from stream-type chinook from central Idaho had prehatch 87Sr/86Sr ratios ???0.711, indicating that a maternal marine Sr isotopic signature is not preserved after the ???1000- to 1400-km migration from the Pacific Ocean. 87Sr/86Sr ratios in the outer portions of otoliths from these Idaho juveniles were similar to those of their respective streams (???0.708-0.722). For Skagit juveniles, fresh water growth was marked by small decreases in otolith Sr/Ca, with increases in Sr/Ca corresponding to increases in 87Sr/86Sr with migration into salt water. Otoliths of Idaho fish had Sr/Ca radial variation patterns that record seasonal fluctuation in ambient water Sr/Ca ratios. The ion microprobe's ability to measure both 87Sr/86Sr and Sr/Ca ratios of otoliths at high spatial resolution in situ provides a new tool for studies of fish rearing and migration. ?? 2004 NRC Canada.

Fabrication of wear-resistant silicon microprobe tips for high-speed surface roughness scanning devices

NASA Astrophysics Data System (ADS)

Wasisto, Hutomo Suryo; Yu, Feng; Doering, Lutz; Völlmeke, Stefan; Brand, Uwe; Bakin, Andrey; Waag, Andreas; Peiner, Erwin

2015-05-01

Silicon microprobe tips are fabricated and integrated with piezoresistive cantilever sensors for high-speed surface roughness scanning systems. The fabrication steps of the high-aspect-ratio silicon microprobe tips were started with photolithography and wet etching of potassium hydroxide (KOH) resulting in crystal-dependent micropyramids. Subsequently, thin conformal wear-resistant layer coating of aluminum oxide (Al2O3) was demonstrated on the backside of the piezoresistive cantilever free end using atomic layer deposition (ALD) method in a binary reaction sequence with a low thermal process and precursors of trimethyl aluminum and water. The deposited Al2O3 layer had a thickness of 14 nm. The captured atomic force microscopy (AFM) image exhibits a root mean square deviation of 0.65 nm confirming the deposited Al2O3 surface quality. Furthermore, vacuum-evaporated 30-nm/200-nm-thick Au/Cr layers were patterned by lift-off and served as an etch mask for Al2O3 wet etching and in ICP cryogenic dry etching. By using SF6/O2 plasma during inductively coupled plasma (ICP) cryogenic dry etching, micropillar tips were obtained. From the preliminary friction and wear data, the developed silicon cantilever sensor has been successfully used in 100 fast measurements of 5- mm-long standard artifact surface with a speed of 15 mm/s and forces of 60-100 μN. Moreover, the results yielded by the fabricated silicon cantilever sensor are in very good agreement with those of calibrated profilometer. These tactile sensors are targeted for use in high-aspect-ratio microform metrology.

Quantitative determination of airborne respirable non-fibrous alpha-silicon carbide by x-ray powder diffractometry.

PubMed

Bye, E; Føreland, S; Lundgren, L; Kruse, K; Rønning, R

2009-06-01

The purpose of the present investigation was to establish a method for the determination of airborne respirable non-fibrous silicon carbide (SiC). The main application is within the industrial production of SiC. Due to the complex airborne aerosol mixture of crystalline compounds in the SiC industry, X-ray powder diffractometry was selected as the most appropriate method. Without any international standard material for the respirable fraction of non-fibrous SiC, pure and suitable products from three SiC plants in Norway were selected. These products have a median particle diameter in the range 4.4-5.1 mum. The method is based on thin sample technique, with the dust deposited on a polycarbonate filter. Absorption correction is done by standard procedures with the use of a silver filter, situated below the polycarbonate filter. The diffraction line used for quantitative determination was selected carefully. This was done to avoid interferences from quartz, cristobalite, and graphite, which all are airborne components present in the atmosphere during the industrial process. The instrumental limit of detection for the method is 12 microg. This method has been used to determine airborne non-fibrous SiC in a comprehensive ongoing project in the Norwegian SiC industry for further epidemiological studies. The method is fully applicable for compliance work.

A method based on Monte Carlo simulations and voxelized anatomical atlases to evaluate and correct uncertainties on radiotracer accumulation quantitation in beta microprobe studies in the rat brain

NASA Astrophysics Data System (ADS)

Pain, F.; Dhenain, M.; Gurden, H.; Routier, A. L.; Lefebvre, F.; Mastrippolito, R.; Lanièce, P.

2008-10-01

The β-microprobe is a simple and versatile technique complementary to small animal positron emission tomography (PET). It relies on local measurements of the concentration of positron-labeled molecules. So far, it has been successfully used in anesthetized rats for pharmacokinetics experiments and for the study of brain energetic metabolism. However, the ability of the technique to provide accurate quantitative measurements using 18F, 11C and 15O tracers is likely to suffer from the contribution of 511 keV gamma rays background to the signal and from the contribution of positrons from brain loci surrounding the locus of interest. The aim of the present paper is to provide a method of evaluating several parameters, which are supposed to affect the quantification of recordings performed in vivo with this methodology. We have developed realistic voxelized phantoms of the rat whole body and brain, and used them as input geometries for Monte Carlo simulations of previous β-microprobe reports. In the context of realistic experiments (binding of 11C-Raclopride to D2 dopaminergic receptors in the striatum; local glucose metabolic rate measurement with 18F-FDG and H2O15 blood flow measurements in the somatosensory cortex), we have calculated the detection efficiencies and corresponding contribution of 511 keV gammas from peripheral organs accumulation. We confirmed that the 511 keV gammas background does not impair quantification. To evaluate the contribution of positrons from adjacent structures, we have developed β-Assistant, a program based on a rat brain voxelized atlas and matrices of local detection efficiencies calculated by Monte Carlo simulations for several probe geometries. This program was used to calculate the 'apparent sensitivity' of the probe for each brain structure included in the detection volume. For a given localization of a probe within the brain, this allows us to quantify the different sources of beta signal. Finally, since stereotaxic accuracy is crucial for quantification in most microprobe studies, the influence of stereotaxic positioning error was studied for several realistic experiments in favorable and unfavorable experimental situations (binding of 11C-Raclopride to D2 dopaminergic receptors in the striatum; binding of 18F-MPPF to 5HT1A receptors in the dorsal raphe nucleus).

Abuse of guaifenesin-containing medications generates an excess of a carboxylate salt of beta-(2-methoxyphenoxy)-lactic acid, a guaifenesin metabolite, and results in urolithiasis.

PubMed

Pickens, C L; Milliron, A R; Fussner, A L; Dversdall, B C; Langenstroer, P; Ferguson, S; Fu, X; Schmitz, F J; Poole, E C

1999-07-01

Several urinary calculi were submitted to our institution for compositional analysis. The typical techniques of analysis, polarized light microscopy, electron microprobe analysis, and infrared spectroscopy proved inadequate for a definitive identification. As a result, a more detailed organic analysis was conducted to determine the exact chemical structure of the material. Infrared spectroscopy and mass spectrometric analysis were carried out on the solid material, providing information concerning the functional groups and the molecular mass of the organic constituent and its components. The stone was solubilized in deuterated solvents and analyzed by nuclear magnetic resonance spectroscopy, which resulted in a definitive chemical structure. The spectroscopic analysis indicated that the stones were composed of a calcium salt of beta-(2-methoxyphenoxy)-lactic acid, a metabolite of the pharmaceutical guaifenesin, which is used as an expectorant. Guaifenesin, an expectorant common in over-the-counter cold and allergy remedies, can cause urolithiasis if taken in excess. Discussions with physicians and their patients confirmed that most patients admitted to taking large doses of guaifenesin-containing medications.

Biomineralisation by earthworms - an investigation into the stability and distribution of amorphous calcium carbonate.

PubMed

Hodson, Mark E; Benning, Liane G; Demarchi, Bea; Penkman, Kirsty E H; Rodriguez-Blanco, Juan D; Schofield, Paul F; Versteegh, Emma A A

Many biominerals form from amorphous calcium carbonate (ACC), but this phase is highly unstable when synthesised in its pure form inorganically. Several species of earthworm secrete calcium carbonate granules which contain highly stable ACC. We analysed the milky fluid from which granules form and solid granules for amino acid (by liquid chromatography) and functional group (by Fourier transform infrared (FTIR) spectroscopy) compositions. Granule elemental composition was determined using inductively coupled plasma-optical emission spectroscopy (ICP-OES) and electron microprobe analysis (EMPA). Mass of ACC present in solid granules was quantified using FTIR and compared to granule elemental and amino acid compositions. Bulk analysis of granules was of powdered bulk material. Spatially resolved analysis was of thin sections of granules using synchrotron-based μ-FTIR and EMPA electron microprobe analysis. The milky fluid from which granules form is amino acid-rich (≤ 136 ± 3 nmol mg -1 (n = 3; ± std dev) per individual amino acid); the CaCO 3 phase present is ACC. Even four years after production, granules contain ACC. No correlation exists between mass of ACC present and granule elemental composition. Granule amino acid concentrations correlate well with ACC content (r ≥ 0.7, p ≤ 0.05) consistent with a role for amino acids (or the proteins they make up) in ACC stabilisation. Intra-granule variation in ACC (RSD = 16%) and amino acid concentration (RSD = 22-35%) was high for granules produced by the same earthworm. Maps of ACC distribution produced using synchrotron-based μ-FTIR mapping of granule thin sections and the relative intensity of the ν 2 : ν 4 peak ratio, cluster analysis and component regression using ACC and calcite standards showed similar spatial distributions of likely ACC-rich and calcite-rich areas. We could not identify organic peaks in the μ-FTIR spectra and thus could not determine whether ACC-rich domains also had relatively high amino acid concentrations. No correlation exists between ACC distribution and elemental concentrations determined by EMPA. ACC present in earthworm CaCO 3 granules is highly stable. Our results suggest a role for amino acids (or proteins) in this stability. We see no evidence for stabilisation of ACC by incorporation of inorganic components. Graphical abstractSynchrotron-based μ-FTIR mapping was used to determine the spatial distribution of amorphous calcium carbonate in earthworm-produced CaCO 3 granules.

Fluoride concentration in dentine as a biomarker of fluoride intake in European roe deer (Capreolus capreolus) - an electron-microprobe study.

PubMed

Richter, Heiko; Kierdorf, Uwe; Richards, Alan; Melcher, Frank; Kierdorf, Horst

2011-08-01

Fluoride concentration in dentine has been recommended as the best marker for the level of chronic fluoride intake and the most suitable indicator of an individual's total body burden of fluoride. We analysed fluoride concentrations in the dentine of cheek teeth of European roe deer from fluoride-polluted habitats to retrospectively assess the level of fluoride uptake into the tissue. Thereby, we tested the hypothesis of the existence of mechanisms that limit fluoride intake of individuals and fluoride exposure of forming dental hard tissues during the late foetal and early postnatal periods in the species. Using electron-microprobe analysis, fluoride profiles were obtained on sectioned P(4)s, M(1)s, and M(3)s from individuals exhibiting pronounced dental fluorosis. Fluoride concentrations were compared between early formed (peripheral) and late-formed (juxtapulpal) dentine both within single teeth and amongst the three different teeth studied. Peripheral dentine of the M(1), which is formed during the late foetal and early postnatal periods, exhibited markedly lower fluoride concentrations than juxtapulpal dentine of the same tooth and both, peripheral and juxtapulpal dentine of P(4) and M(3) that are formed post-weaning. Our study provides strong support for the hypothesis that in the European roe deer the prenatal and early postnatal (pre-weaning) stages of dental development are (largely) protected against exposure to excess fluoride. This is attributed to the operation of certain protective mechanisms during these periods. Copyright © 2011 Elsevier Ltd. All rights reserved.

Olivine-melt relationships and syneruptive redox variations in the 1959 eruption of K$$\\bar{i}$$lauea Volcano as revealed by XANES

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

Helz, R. T.; Cottrell, E.; Brounce, M. N.

The 1959 summit eruption of Kmore » $$\\bar{i}$$lauea Volcano exhibited high lava fountains of gas-rich, primitive magma, containing olivine + chromian spinel in highly vesicular brown glass. Microprobe analysis of these samples shows that euhedral rims on olivine phenocrysts, in direct contact with glass, vary significantly in forsterite (Fo) content, at constant major-element melt composition, as do unzoned groundmass olivine crystals. Ferric/total iron (Fe+ 3/FeT)ratios for matrix and interstitial glasses, plus olivine-hosted glass inclusions in eight 1959 scoria samples have been determined by micro X-ray absorption near-edge structure spectroscopy (μ-XANES). These data show that much of the variation in Fo content reflects variation in oxidation state of iron in the melt, which varies with sulfur concentration in the glass and (locally) with proximity to scoria edges in contact with air. Data for 24 olivine-melt pairs in the better-equilibrated samples from later in the eruption show KD averaging 0.280 ± 0.03 for the exchange of Fe and Mg between olivine and melt, somewhat displaced from the value of 0.30 ± 0.03 given by Roeder and Emslie (1970). This may reflect the low SiO2 content of the 1959 magmas, which is lower than that in most K$$\\bar{i}$$lauea tholeiites. More broadly, we show the potential of μ-XANES and electron microprobe to revisit and refine the value of KD in natural systems.« less

Approximate chemical analysis of volcanic glasses using Raman spectroscopy

PubMed Central

Morgavi, Daniele; Hess, Kai‐Uwe; Neuville, Daniel R.; Borovkov, Nikita; Perugini, Diego; Dingwell, Donald B.

2015-01-01

The effect of chemical composition on the Raman spectra of a series of natural calcalkaline silicate glasses has been quantified by performing electron microprobe analyses and obtaining Raman spectra on glassy filaments (~450 µm) derived from a magma mingling experiment. The results provide a robust compositionally‐dependent database for the Raman spectra of natural silicate glasses along the calcalkaline series. An empirical model based on both the acquired Raman spectra and an ideal mixing equation between calcalkaline basaltic and rhyolitic end‐members is constructed enabling the estimation of the chemical composition and degree of polymerization of silicate glasses using Raman spectra. The model is relatively insensitive to acquisition conditions and has been validated using the MPI‐DING geochemical standard glasses1 as well as further samples. The methods and model developed here offer several advantages compared with other analytical and spectroscopic methods such as infrared spectroscopy, X‐ray fluorescence spectroscopy, electron and ion microprobe analyses, inasmuch as Raman spectroscopy can be performed with a high spatial resolution (1 µm2) without the need for any sample preparation as a nondestructive technique. This study represents an advance in efforts to provide the first database of Raman spectra for natural silicate glasses and yields a new approach for the treatment of Raman spectra, which allows us to extract approximate information about the chemical composition of natural silicate glasses using Raman spectroscopy. We anticipate its application in handheld in situ terrestrial field studies of silicate glasses under extreme conditions (e.g. extraterrestrial and submarine environments). © 2015 The Authors Journal of Raman Spectroscopy Published by John Wiley & Sons Ltd PMID:27656038

A comparative study of quantitative microsegregation analyses performed during the solidification of the Ni-base superalloy CMSX-10

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

Seo, Seong-Moon, E-mail: castme@kims.re.kr; Jeong, Hi-Won; Ahn, Young-Keun

Quantitative microsegregation analyses were systematically carried out during the solidification of the Ni-base superalloy CMSX-10 to clarify the methodological effect on the quantification of microsegregation and to fully understand the solidification microstructure. Three experimental techniques, namely, mushy zone quenching (MZQ), planar directional solidification followed by quenching (PDSQ), and random sampling (RS), were implemented for the analysis of microsegregation tendency and the magnitude of solute elements by electron probe microanalysis. The microprobe data and the calculation results of the diffusion field ahead of the solid/liquid (S/L) interface of PDSQ samples revealed that the liquid composition at the S/L interface is significantlymore » influenced by quenching. By applying the PDSQ technique, it was also found that the partition coefficients of all solute elements do not change appreciably during the solidification of primary γ. All three techniques could reasonably predict the segregation behavior of most solute elements. Nevertheless, the RS approach has a tendency to overestimate the magnitude of segregation for most solute elements when compared to the MZQ and PDSQ techniques. Moreover, the segregation direction of Cr and Mo predicted by the RS approach was found to be opposite from the results obtained by the MZQ and PDSQ techniques. This conflicting segregation behavior of Cr and Mo was discussed intensively. It was shown that the formation of Cr-rich areas near the γ/γ′ eutectic in various Ni-base superalloys, including the CMSX-10 alloy, could be successfully explained by the results of microprobe analysis performed on a sample quenched during the planar directional solidification of γ/γ′ eutectic. - Highlights: • Methodological effect on the quantification of microsegregation was clarified. • The liquid composition at the S/L interface was influenced by quenching. • The segregation direction of Cr varied depending on the experimental techniques. • Cr and Mo segregation in Ni-base superalloys was fully understood.« less

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

Macente, A.; Fusseis, F.; Menegon, L.

Reaction and deformation microfabrics provide key information to understand the thermodynamic and kinetic controls of tectono-metamorphic processes, however they are usually analysed in two dimensions, omitting important information regarding the third spatial dimension. We applied synchrotron-based X-ray microtomography to document the evolution of a pristine olivine gabbro into a deformed omphacite-garnet eclogite in four dimensions, where the 4th dimension is represented by the degree of strain. In the investigated samples, which cover a strain gradient into a shear zone from the Western Gneiss Region (Norway), we focused on the spatial transformation of garnet coronas into elongated clusters of garnets withmore » increasing strain. Our microtomographic data allowed quantification of garnet volume, shape and spatial arrangement evolution with increasing strain. We combined microtomographic observations with light microscope- and backscatter electron images as well as electron microprobe- (EMPA) and electron backscatter diffraction (EBSD) analysis to correlate mineral composition and orientation data with the X-ray absorption signal of the same mineral grains. With increasing deformation, the garnet volume almost triples. In the low strain domain, garnets form a well interconnected large garnet aggregate that develops throughout the entire Page 1 of 52 sample. We also observed that garnet coronas in the gabbros never completely encapsulate olivine grains. In the most highly deformed eclogites, the oblate shapes of garnet clusters reflect a deformational origin of the microfabrics. We interpret the aligned garnet aggregates to direct synkinematic fluid flow and consequently influence the transport of dissolved chemical components. EBSD analyses reveal that garnet show a near-random crystal preferred orientation that testifies no evidence for crystal plasticity. There is, however evidence for minor fracturing, neo-nucleation and overgrowth. Microprobe chemical analysis revealed that garnet compositions progressively equilibrate to eclogite facies, becoming more almandine-rich. We interpret these observations as pointing to a mechanical disintegration of the garnet coronas during strain localisation, and their rearrangement into individual garnet clusters through a combination of garnet coalescence and overgrowth while the rock was deforming.« less

Magmatic-hydrothermal fluid interaction and mineralization in alkali-syenite nodules from the Breccia Museo pyroclastic deposit, Naples, Italy: Chapter 7 in Volcanism in the Campania Plain — Vesuvius, Campi Flegrei and Ignimbrites

USGS Publications Warehouse

Fedele, Luca; Tarzia, Maurizio; Belkin, Harvey E.; De Vivo, Benedetto; Lima, Annamaria; Lowenstern, Jacob

2007-01-01

The Breccia Museo, a pyroclastic flow that crops out in the Campi Flegrei volcanic complex (Naples, Italy), contains alkali-syenite (trachyte) nodules with enrichment in Cl and incompatible elements (e.g., U, Zr, Th, and rare-earth elements). Zircon was dated at ≈52 ka, by U-Th isotope systematics using a SHRIMP. Scanning electron microscope and electron microprobe analysis of the constituent phases have documented the mineralogical and textural evolution of the nodules of feldspar and mafic accumulations on the magma chamber margins. Detailed electron microprobe data are given for alkali and plagioclase feldspar, salite to ferrosalite clinopyroxene, pargasite, ferrogargasite, magnesio-hastingsite hornblende amphibole, biotite mica, Cl-rich scapolite, and a member (probable davyne-type) of the cancrinite group. Detailed whole rock, major and minor element data are also presented for selected nodules. A wide variety of common and uncommon accessory minerals were identified such as zircon, baddeleyite, zirconolite, pollucite, sodalite, titanite, monazite, cheralite, apatite, titanomagnetite and its alteration products, scheelite, ferberite, uraninite/thorianite, uranpyrochlore, thorite, pyrite, chalcopyrite, and galena. Scanning electron microscope analysis of opened fluid inclusions identified halite, sylvite, anhydrite, tungstates, carbonates, silicates, sulfides, and phosphates; most are probably daughter minerals. Microthermometric determinations on secondary fluid inclusions hosted by alkali feldspar define a temperature regime dominated by hypersaline aqueous fluids. Fluid-inclusion temperature data and mineral-pair geothermometers for coexisting feldspars and hornblende and plagioclase were used to construct a pressure-temperature scenario for the development and evolution of the nodules. We have compared the environment of porphyry copper formation and the petrogenetic environment constructed for the studied nodules. The suite of ore minerals observed in the nodules supports a potential for mineralization, which is similar to that observed in the alkaline volcanic systems of southern Italy (Pantelleria, Pontine Archipelago, Mt. Somma-Vesuvius).

Characterization of flux-grown Trace-element-doped titanite using the high-mass-resolution ion microprobe (SHRIMP-RG)

USGS Publications Warehouse

Mazdab, F.K.

2009-01-01

Crystals of titanite can be readily grown under ambient pressure from a mixture of CaO, TiO2 and SiO2 in the presence of molten sodium tetraborate. The crystals produced are euhedral and prismatic, lustrous and transparent, and up to 5 mm in length. Titanite obtained by this method contains approximately 4300 ppm Na and 220 ppm B contributed from the flux. In addition to dopant-free material, titanite containing trace alkali and alkaline earth metals (K, Sr, Ba), transition metals (Sc, Cr, Ni, Y, Zr, Nb, Hf and Ta), rare-earth elements (REE), actinides (Th, U) and p-block elements (F, S, Cl, Ge, Sn and Pb) have been prepared using the same procedure. Back-scattered electron (BSE) imaging accompanied by ion-microprobe (SHRIMP-RG) analysis confirms significant incorporation of selected trace-elements at structural sites. Regardless of some zonation, the large size of the crystals and broad regions of chemical homogeneity make these crystals useful as experimental starting material, and as matrix-matched trace-element standards for a variety of microbeam analytical techniques where amorphous titanite glass, heterogeneous natural titanite or a non-titanite standard may be less than satisfactory. Trace-element-doped synthetic crystals can also provide a convenient proxy for a better understanding of trace-element incorporation in natural titanite. Comparisons with igneous, authigenic and high-temperature metasomatic titanite are examined. The use of high-mass-resolution SIMS also demonstrates the analytical challenges inherent to any in situ mass-spectrometry-based analysis of titanite, owing to the production of difficult-to-resolve molecular interferences. These interferences are dominated by Ca-Ca, Ca-Ti and Ti-Ti dimers that are significant in the mass range of 80-100, affecting all isotopes of Sr and Zr, as well as 89Y and 93Nb. Methods do exist for the evaluation of interferences by these dimers and of polyatomic interferences on the LREE.

Otolith oxygen isotopes measured by high-precision secondary ion mass spectrometry reflect life history of a yellowfin sole (Limanda aspera).

PubMed

Matta, Mary Elizabeth; Orland, Ian J; Ushikubo, Takayuki; Helser, Thomas E; Black, Bryan A; Valley, John W

2013-03-30

The oxygen isotope ratio (δ(18)O value) of aragonite fish otoliths is dependent on the temperature and the δ(18)O value of the ambient water and can thus reflect the environmental history of a fish. Secondary ion mass spectrometry (SIMS) offers a spatial-resolution advantage over conventional acid-digestion techniques for stable isotope analysis of otoliths, especially given their compact nature. High-precision otolith δ(18)O analysis was conducted with an IMS-1280 ion microprobe to investigate the life history of a yellowfin sole (Limanda aspera), a Bering Sea species known to migrate ontogenetically. The otolith was cut transversely through its core and one half was roasted to eliminate organic contaminants. Values of δ(18)O were measured in 10-µm spots along three transects (two in the roasted half, one in the unroasted half) from the core toward the edge. Otolith annual growth zones were dated using the dendrochronology technique of crossdating. Measured values of δ(18)O ranged from 29.0 to 34.1‰ (relative to Vienna Standard Mean Ocean Water). Ontogenetic migration from shallow to deeper waters was reflected in generally increasing δ(18)O values from age-0 to approximately age-7 and subsequent stabilization after the expected onset of maturity at age-7. Cyclical variations of δ(18)O values within juvenile otolith growth zones, up to 3.9‰ in magnitude, were caused by a combination of seasonal changes in the temperature and the δ(18)O value of the ambient water. The ion microprobe produced a high-precision and high-resolution record of the relative environmental conditions experienced by a yellowfin sole that was consistent with population-level studies of ontogeny. Furthermore, this study represents the first time that crossdating has been used to ensure the dating accuracy of δ(18)O measurements in otoliths. Copyright © 2013 John Wiley & Sons, Ltd.

Growth and properties of oxygen- and ion-doped Bi2Sr2CaCu2O8+δ single crystals

NASA Astrophysics Data System (ADS)

Mitzi, D. B.; Lombardo, L. W.; Kapitulnik, A.; Laderman, S. S.; Jacowitz, R. D.

1990-04-01

A directional solidification method for growing large single crystals in the Bi2Sr2CaCu2O8+δ system is reported. Ion doping, with replacement of La for Sr and Y for Ca, as well as oxygen doping in these crystals has been explored. Doped and undoped crystals have been characterized using microprobe analysis, x-ray diffraction, thermogravimetric analysis, and magnetic and Hall measurements. Ion doping results in little change of the superconducting transition for substitution levels below 20-25%, while beyond this level the Meissner signal broadens and the low-temperature Meissner signal decreases. Microprobe analysis and x-ray diffraction performed on these more highly substituted single crystals provide evidence for inhomogeneity and phase segregation into regions of distinct composition. Annealing unsubstituted crystals in increasing partial pressures of oxygen reversibly depresses the superconducting transition temperature from 90 (as made) to 77 K (oxygen pressure annealed), while the carrier concentrations, as determined from Hall effect measurements, increase from n=3.1(3)×1021 cm-3 (0.34 holes per Cu site) to 4.6(3)×1021 cm-3 (0.50 holes per Cu site). No degradation of the Meissner transition or other indications of inhomogeneity or phase segregation with doping are noted, suggesting that oxygen-doped Bi2Sr2CaCu2O8+δ is a suitable system for pursuing doping studies. The decrease in Tc with concentration for 0.34<=n<=0.50 indicates that a high-carrier-concentration regime exists in which Tc decreases with n and suggests that this decrease does not arise from material inhomogeneity or other materials problems. An examination of the variation of Tc with the density of states and lattice constants for all of the doped and undoped superconducting samples considered here indicates that changes in Tc with doping are primarily affected by changes in the density of states (or carrier concentration) rather than by structural variation induced by the doping.

Strength Characteristics of Resorbable Osteoconductive Ceramics Based on Diphosphates of Calcium and Alkali Metals

NASA Astrophysics Data System (ADS)

Putlayev, V. I.; Evdokimov, P. V.; Garshev, A. V.; Prosvirin, D. V.; Klimashina, E. S.; Safronova, T. V.; Ivanov, V. K.

2014-02-01

An investigation into the strength characteristics of ceramics based on diphosphates Ca(3- x)М2 x (PO4)2 ( x = 0-1 and М = Na, K) provides evidence of composition strengthening in the range х = 0.6-0.8 containing the greatest amount of the supercooled high-temperature modification α-СаМРО4. The method of high-temperature x-ray diffractometry is used to examine thermal expansion of rhenanite phases of СаМРО4.

Molecular beam epitaxial growth and structural characterization of ZnS on (001) GaAs

NASA Technical Reports Server (NTRS)

Benz, R. G., II; Huang, P. C.; Stock, S. R.; Summers, C. J.

1988-01-01

The effect of surface nucleation processes on the quality of ZnS layers grown on (001) GaAs substrates by molecular beam epitaxy is reported. Reflection high energy electron diffraction indicated that nucleation at high temperatures produced more planar surfaces than nucleation at low temperatures, but the crystalline quality as assessed by X-ray double crystal diffractometry is relatively independent of nucleation temperature. A critical factor in layer quality was the initial roughness of the GaAs surfaces.

A Study of the Oscillation Marks' Characteristics of Continuously Cast Incoloy Alloy 825 Blooms

NASA Astrophysics Data System (ADS)

Saleem, Saud; Vynnycky, Michael; Fredriksson, Hasse

2016-08-01

A comprehensive experimental study of oscillation mark (OM) formation and its characteristics during the solidification of Incoloy alloy 825 in the continuous casting of blooms is investigated by plant trials and metallographic study. The experiments involved two heats with the same casting and mold conditions and sampling at different locations across the strand. The metallographic study combined macro/micro-examinations of OMs and segregation analysis of Cr, Mn, Mo, Ni, and Si by microprobe analysis. The results show that OMs have widely different characteristics, such as mark type, depth, segregation, and accompanying microstructure. Furthermore, the mark pitch can vary considerably even for the similar casting conditions, leading to different conditions for the marks' formation in relation to the mold's cyclic movement. Finally, a mechanism for the OM formation is discussed and proposed. Possible solutions for minimizing the observed defects by optimizing the mold conditions are suggested.

The trace element chemistry of CaS in enstatite chondrites and some implications regarding its origin

NASA Technical Reports Server (NTRS)

Larimer, John W.; Ganapathy, R.

1987-01-01

The trace element distribution in oldhamite (CaS) extracted from enstatite chondrites was determined by INAA. Prior to extraction, the petrologic setting of the grains was studied microscopically, and their minor element contents determined by microprobe analysis; samples that displayed a wide range of minor element contents were selected for detailed elementary analysis. Those samples of CaS suspected to be more primitive on the basis of their minor element and petrologic siting contain the entire inventory of the host meteorite's light REE (LREE) and Eu, plus 30-50 percent of the heavy-REE inventory. In less primitive samples, the LREE are less enriched although Eu remains highly concentrated. Several other elements, including lithophiles and chalcophiles, are most enriched in the most primitive CaS. It is suggested that oldhamite played a key role in the redistribution of these elements during the metamorphism and evolution of enstatite-rich material.

Some wear studies on aircraft brake systems

NASA Technical Reports Server (NTRS)

Ho, T. L.

1975-01-01

An initial investigation of worn surfaces in friction pads and steel rotors used in current aircraft brakes was carried out using electron microprobe and X-ray diffraction analysis. It consists of the topographical study and the analysis of chemical element distribution. Based upon this initial examination, two approaches, microscopic and macroscopic have been conducted to interpret and formulate the wear mechanism of the aircraft brake materials. Microscopically, the wear particles were examined. The initiation and growth of surface cracks and the oxidation were emphasized in this investigation. Macroscopically, it has been found that, for the current copper based brake material sliding against 17-22 AS steel in a caliper brake, the surface temperature raised due to frictional heat is nonlinearly proportional to the load applied and slide time with speed at 1750 rpm. The wear of brake materials is then proportional to this temperature and is also a function of the melting temperature for copper.

The identification of group II inclusions in carbonaceous chondrites by electron probe microanalysis of perovskite

NASA Technical Reports Server (NTRS)

Kornacki, A. S.; Wood, J. A.

1985-01-01

The technique developed by Kornacki (1984) for identifying group II Ca/Al-rich inclusions in carbonaceous chondrites by electron-microprobe analysis of the ZrO2 or Y2O3 content of their perovskite component is demonstrated using material from 20 Allende inclusions. The results are presented in tables and graphs and compared with findings obtained by other procedures. Group II inclusions are found to have perovskites generally containing less than 0.10 wt pct ZrO2 and/or Y2O3 (average of several grains), while those of groups I, III, V, and VI have more than 0.25 wt pct ZrO2. Analysis of data on eight Allende Ca/Al-rich inclusions shows that 75 percent of the fine-grained inclusions belong to group II. The implications of these findings for fractionation processes in the primitive solar nebula are indicated.

Trace element abundance determinations by Synchrotron X Ray Fluorescence (SXRF) on returned comet nucleus mineral grains

NASA Technical Reports Server (NTRS)

Flynn, G. J.; Sutton, S. R.

1989-01-01

Trace element analyses were performed on bulk cosmic dust particles by Proton Induced X Ray Emission (PIXE) and Synchrotron X Ray Fluorescence (SXRF). When present at or near chondritic abundances the trace elements K, Ti, Cr, Mn, Cu, Zn, Ga, Ge, Se, and Br are presently detectable by SXRF in particles of 20 micron diameter. Improvements to the SXRF analysis facility at the National Synchrotron Light Source presently underway should increase the range of detectable elements and permit the analysis of smaller samples. In addition the Advanced Photon Source will be commissioned at Argonne National Laboratory in 1995. This 7 to 8 GeV positron storage ring, specifically designed for high-energy undulator and wiggler insertion devices, will be an ideal source for an x ray microprobe with one micron spatial resolution and better than 100 ppb elemental sensitivity for most elements. Thus trace element analysis of individual micron-sized grains should be possible by the time of the comet nucleus sample return mission.

Probing below the Surface of Mars. ITEA/NASA-JPL Learning Activity.

ERIC Educational Resources Information Center

Urquhart, Mary; Urquhart, Sally

2000-01-01

This activity, developed by NASA's Jet Propulsion Laboratory, involves students in recording and graphing temperature data to learn about NASA's Mars Microprobe Mission, Deep Space 2, and how the properties of a material affect the transfer of heat. (Author/JOW)

Compositional Zoning and Mn-Cr Systematics in Carbonates from the Y791198 CM2 Carbonaceous Chondrite

NASA Technical Reports Server (NTRS)

Brearley, Adrian J.; Hutcheon, Ian D.; Browning, Lauren

2001-01-01

Cathodoluminescence and microprobe analyses show that carbonates in Y791198 exhibit complex zoning. Cr-Mn dating suggests formation of carbonates 10 Ma after CAI formation Additional information is contained in the original extended abstract..

High Fluence Synchrotron Radiation Microprobe Effects on Stardust Interstellar Dust Candidates

NASA Astrophysics Data System (ADS)

Simionovici, A.; Allen, C.; Bajt, S.; Bastien, R.; Bechtel, H.; Borg, J.; Brenker, F. E.; Bridges, J. C.; Brownlee, D. E.; Burchell, M. J.; Burghammer, M.; Butterworth, A.; Cloetens, P.; Davis, A. M.; Floss, C.; Flynn, G.; Frank, D.; Gainsforth, Z.; Grün, E.; Heck, P. R.; Hillier, J.; Hoppe, P.; Howard, L.; Huss, G. R.; Huth, J.; Kearsley, A. T.; King, A. J.; Lai, B.; Leitner, J.; Lemelle, L.; Leroux, H.; Lettieri, R.; Marchant, W.; Nittler, L.; Ogliore, R.; Postberg, F.; Sandford, S.; Sans Tresseras, J. A.; Schoonjans, T.; Schmitz, S.; Silversmit, G.; Srama, R.; Stadermann, F. J.; Stephan, T.; Stodolna, J.; Stroud, R. M.; Sutton, S.; Tucoulou, R.; Trieloff, M.; Tsou, P.; Tsuchiyama, A.; Tyliczszak, T.; Vekemans, B.; Vincze, L.; Westphal, A. J.; Zevin, D.; Zolensky, M. E.; 29,000 Stardust@Home Dusters

2011-03-01

We are presenting for the first time damage effects produced by focused high-fluence synchrotron beams on Stardust interstellar dust candidates. The damage produced on submicrometer grains shows up as particle smearing. We attribute this mainly to charging effects.

Particulate matter in exhaled breath condensate: A promising indicator of environmental conditions

NASA Astrophysics Data System (ADS)

Pinheiro, Teresa; Alexandra Barreiros, M.; Alves, Luis C.; Felix, Pedro M.; Franco, Cristiana; Sousa, Joana; Almeida, S. M.

2011-10-01

Assessing the retention of aerosol particles in the human lung, one of the most important pathways of absorption, is a demanding issue. At present, there is no direct biomarker of exposure for the respiratory system. The collection of exhaled breath condensate (EBC) constitutes a new non-invasive method for sampling from the lung. However, the heterogeneity of the sample due to particulate matter suspended in the condensed phase may influence the quality of analytical results in occupational assessments. The main objective of the study was to confirm the presence of particulate matter in the condensate, to investigate how large the particles in suspension could be and to determine their elemental contents relative to those of EBC matrix. This paper reports on preliminary nuclear microprobe data of particulate matter in EBC. The sizes and the elemental contents of particles suspended in EBC of workers of a lead processing industry and in EBC of non-exposed individuals were inspected. Results demonstrated that EBC of workers contain large aerosol particles, isolated and in agglomerates, contrasting with non-exposed individuals. The particles contained high concentrations of Cl, Ca, Zn and Pb that are elements associated to the production process. These elements were also present in the EBC matrix although in much lower levels, suggesting that a fraction of the inhaled particulate matter was solubilised or their size-ranges were below the nuclear microprobe resolution. Therefore, the morphological characterization of individual particles achieved with nuclear microprobe techniques helped describing EBC constituents in detail, to comprehend their origin and enabled to delineate methodological procedures that can be recommended in occupational assessments. These aspects are critical to the validation of EBC as a biomarker of exposure to metals for the respiratory system.

Functional group and individual maceral chemistry of high volatile bituminous coals from southern Indiana: Controls on coking

USGS Publications Warehouse

Walker, R.; Mastalerz, Maria

2004-01-01

The individual maceral chemistries of two Pennsylvanian, high volatile bituminous coals, the Danville Coal Member (Dugger Formation, R o=0.55%) and the Lower Block Coal Member (Brazil Formation, R o=0.56%) of Indiana, were investigated using electron microprobe and Fourier Transform Infrared Spectrometry (FTIR) techniques, with the purpose of understanding differences in their coking behavior. Microprobe results reveal that carbon contents are highest in inertinite and sporinite, followed by desmocollinite and telocollinite. Oxygen and organic nitrogen are most abundant in telocollinite and desmocollinite; sporinite and inertinite contain lesser amounts of these two elements. Organic sulfur contents are highest in sporinite, lowest in inertinite, and intermediate in desmocollinite and telocollinite. Vitrinites within the Danville and Lower Block coals are very similar in elemental composition, while Lower Block inertinites and sporinites have higher carbon, lower oxygen, and sulfur contents which, when combined with the inertinite-and sporinite-rich composition of the Lower Block seam, strongly influences its whole coal chemistry. Fourier transform infrared spectrometry revealed greater aromatic hydrogen in the Lower Block coal, along with higher CH2/CH3 ratios, which suggest that liptinites contribute considerable amounts of long-chain, unbranched aliphatics to the overall kerogen composition of the Lower Block coal. Long-chain, unbranched aliphatics crack at higher temperatures, producing tar and oily byproducts during coking; these may help increase Lower Block plasticity. Electron microprobe and FTIR results indicate that individual maceral chemistries, combined with the maceral composition of the seam, are the primary control of better coking properties of the Lower Block coal. ?? 2003 Elsevier B.V. All rights reserved.

A high brightness proton injector for the Tandetron accelerator at Jožef Stefan Institute

NASA Astrophysics Data System (ADS)

Pelicon, Primož; Podaru, Nicolae C.; Vavpetič, Primož; Jeromel, Luka; Ogrinc Potocnik, Nina; Ondračka, Simon; Gottdang, Andreas; Mous, Dirk J. M.

2014-08-01

Jožef Stefan Institute recently commissioned a high brightness H- ion beam injection system for its existing tandem accelerator facility. Custom developed by High Voltage Engineering Europa, the multicusp ion source has been tuned to deliver at the entrance of the Tandetron™ accelerator H- ion beams with a measured brightness of 17.1 A m-2 rad-2 eV-1 at 170 μA, equivalent to an energy normalized beam emittance of 0.767 π mm mrad MeV1/2. Upgrading the accelerator facility with the new injection system provides two main advantages. First, the high brightness of the new ion source enables the reduction of object slit aperture and the reduction of acceptance angle at the nuclear microprobe, resulting in a reduced beam size at selected beam intensity, which significantly improves the probe resolution for micro-PIXE applications. Secondly, the upgrade strongly enhances the accelerator up-time since H and He beams are produced by independent ion sources, introducing a constant availability of 3He beam for fusion-related research with NRA. The ion beam particle losses and ion beam emittance growth imply that the aforementioned beam brightness is reduced by transport through the ion optical system. To obtain quantitative information on the available brightness at the high-energy side of the accelerator, the proton beam brightness is determined in the nuclear microprobe beamline. Based on the experience obtained during the first months of operation for micro-PIXE applications, further necessary steps are indicated to obtain optimal coupling of the new ion source with the accelerator to increase the normalized high-energy proton beam brightness at the JSI microprobe, currently at 14 A m-2 rad-2 eV-1, with the output current at 18% of its available maximum.

Ion microprobe elemental analyses of impact features on interplanetary dust experiment sensor surfaces

NASA Technical Reports Server (NTRS)

Simon, Charles G.; Hunter, Jerry L.; Wortman, Jim J.; Griffis, Dieter P.

1992-01-01

Hypervelocity impact features from very small particles (less than 3 microns in diameter) on several of the electro-active dust sensors used in the Interplanetary Dust Experiment (IDE) were subjected to elemental analysis using an ion microscope. The same analytical techniques were applied to impact and containment features on a set of ultra-pure, highly polished single crystal germanium wafer witness plates that were mounted on tray B12. Very little unambiguously identifiable impactor debris was found in the central craters or shatter zones of small impacts in this crystalline surface. The surface contamination, ubiquitous on the surface of the Long Duration Exposure Facility, has greatly complicated data collection and interpretation from microparticle impacts on all surfaces.

Chemical processes involved in the initiation of hot corrosion of B-1900 and NASA-TRW VIA

NASA Technical Reports Server (NTRS)

Fryburg, G. C.; Kohl, F. J.; Stearns, C. A.

1979-01-01

Sodium sulfate induced hot corrosion of B-1900 and NASA-TRW VIA at 900 C was studied with special emphasis on the chemical reactions occurring during and immediately after the induction period. Thermogravimetric tests were run for set periods of time after which the samples were washed with water and water soluable metal salts and/or residual sulfates were analyzed chemically. Element distributions within the oxide layer were obtained from electron microprobe X-ray micrographs. A third set of samples were subjected to surface analysis by X-ray photoelectron spectroscopy. Evolution of SO2 was monitored throughout many of the hot corrosion tests. Results are interpreted in terms of acid-base fluxing mechanisms.

Inhomogeneities and segregation behavior in strontium—barium niobate fibers grown by laser-heated pedestal growth technique. Part II

NASA Astrophysics Data System (ADS)

Erdei, S.; Galambos, L.; Tanaka, I.; Hesselink, L.; Cross, L. E.; Feigelson, R. S.; Ainger, F. W.; Kojima, H.

1996-10-01

Inhomogeneities in Ce-doped and undoped fibers grown by laser-heated pedestal growth (LHPG) along the c- or a- axis were investigated by two-dimensional scanning electron microprobe analysis (SEPMA). SEPMA data indicated that these cores are primarily connected with the source rod compositions utilized and the convection characteristics of the LHPG technique. Ba enrichment and Sr decrease were primarily detected in the cores and qualitatively described in terms of the composition-control mechanism of LHPG, the complex-segregation and a modified Burton—Prim—Slichter (BPS) equation. Certain aspects of defect structure as a complex congruency related phenomenon are also discussed in the paper giving a more complete interpretation of the origin of cores in SBN fibers.

Matrix and fine-grained rims in the unequilibrated CO3 chondrite, ALHA77307 - Origins and evidence for diverse, primitive nebular dust components

NASA Technical Reports Server (NTRS)

Brearley, Adrian J.

1993-01-01

SEM, TEM, and electron microprobe analysis were used to investigate in detail the mineralogical and chemical characteristics of dark matrix and fine-grained rims in the unequilibrated CO3 chondrite ALHA77307. Data obtained revealed that there was a remarkable diversity of distinct mineralogical components, which can be identified using their chemical and textural characteristics. The matrix and rim components in ALHA77307 formed by disequilibrium condensation process as fine-grained amorphous dust that is represented by the abundant amorphous component in the matrix. Subsequent thermal processing of this condensate material, in a variety of environments in the nebula, caused partial or complete recrystallization of the fine-grained dust.

High-resolution EPMA X-ray images of mother liquid inclusions in a Pd2Ga single crystal

NASA Astrophysics Data System (ADS)

Müller, D.; Schwerin, J.; Gille, P.; Fehr, K. T.

2014-03-01

During crystal growth from solution inclusions of different compositions were trapped at the rim of a Pd2Ga single crystal. Their fine-grained (< 5 μm) internal structure demands special requirements for electron microprobe analysis, realized by low-voltage (5 keV) element mapping applying a step size of 0.138 μm for each pixel. It can be shown, that these inclusions represent an isolated chemical system, and that crystallisation upon cooling follows the expected thermodynamic phase relations. Thus the final composition in the centre of the inclusion consists of a small-scale mixture of PdGa and Pd5Ga3 evolved out of a solid-solid decomposition of Pd5Ga4.

Rare Earth Element Partition Coefficients from Enstatite/Melt Synthesis Experiments

NASA Technical Reports Server (NTRS)

Schwandt, Craig S.; McKay, Gordon A.

1997-01-01

Enstatite (En(80)Fs(19)Wo(01)) was synthesized from a hypersthene normative basaltic melt doped at the same time with La, Ce, Nd, Sm, Eu, Dy, Er, Yb and Lu. The rare earth element concentrations were measured in both the basaltic glass and the enstatite. Rare earth element concentrations in the glass were determined by electron microprobe analysis with uncertainties less than two percent relative. Rare earth element concentrations in enstatite were determined by secondary ion mass spectrometry with uncertainties less than five percent relative. The resulting rare earth element partition signature for enstatite is similar to previous calculated and composite low-Ca pigeonite signatures, but is better defined and differs in several details. The partition coefficients are consistent with crystal structural constraints.

Electrochemical and Spectroscopic Analysis of Mg2+ Intercalation into Thin Film Electrodes of Layered Oxides: V2O5 and MoO3

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

Gershinsky, G; Yoo, HD; Gofer, Y

Electrochemical, surface, and structural studies related to rechargeable Mg batteries were carried out with monolithic thin-film cathodes comprising layered V2O5 and MoO3. The reversible intercalation reactions of these electrodes with Mg ion in nonaqueous Mg salt solutions were explored using a variety of analytical tools. These included slow-scan rate cyclic voltammetry (SSCV), chrono-potentiometry (galvanostatic cycling), Raman and photoelectron spectroscopies, high-resolution microscopy, and XRD. The V2O5 electrodes exhibited reversible Mg-ion intercalation at capacities around 150-180 mAh g(-1) with 100% efficiency. A capacity of 220 mAh g(-1) at >95% efficiency was obtained with MoO3 electrodes. By applying the electrochemical driving force sufficientlymore » slowly it was possible to measure the electrodes at equilibrium conditions and verify by spectroscopy, microscopy, and diffractometry that these electrodes undergo fully reversible structural changes upon Mg-ion insertion/deinsertion cycling.« less

Biological pretreatment of corn stover with ligninolytic enzyme for high efficient enzymatic hydrolysis.

PubMed

Wang, Feng-Qin; Xie, Hui; Chen, Wei; Wang, En-Tao; Du, Feng-Guang; Song, An-Dong

2013-09-01

Aiming at increasing the efficiency of transferring corn stover into sugars, a biological pretreatment was developed and investigated in this study. The protocol was characterized by the pretreatment with crude ligninolytic enzymes from Phanerochete chrysosporium and Coridus versicolor to break the lignin structure in corn stover, followed by a washing procedure to eliminate the inhibition of ligninolytic enzyme on cellulase. By a 2 d-pretreatment, sugar yield from corn stover hydrolysis could be increased by 50.2% (up to 323 mg/g) compared with that of the control. X-ray diffractometry and FT-IR analysis revealed that biological pretreatment could partially remove the lignin of corn stover, and consequently enhance the enzymatic hydrolysis efficiency of cellulose and hemeicellulose. In addition, the amount of microbial inhibitors, such as acetic acid and furfural, were much lower in biological pretreatment than that in acid pretreatment. This study provided a promising pretreatment method for biotransformation of corn stovers. Copyright © 2013 Elsevier Ltd. All rights reserved.

Electrochromic Properties of Tungsten Oxide Films Prepared by Reactive Sputtering

NASA Astrophysics Data System (ADS)

Kim, Min Hong; Kang, Tai Young; Jung, Yu Sup; Kim, Kyung Hwan

2013-05-01

WO3-x thin films were deposited on induim tin oxide (ITO) glass substrates with various oxygen flow ratios from 0.55 to 0.7 by the reactive facing-target sputtering method, at a power density of 4 W/cm2 and room temperature. The structural properties of the WO3-x thin films were measured by X-ray diffractometry and Raman spectral analysis. As-deposited WO3-x thin films had an amorphous structure. In the Raman spectra, WO3-x thin films exhibited two strong peaks at 770 and 950 cm-1 attributed to the vibrations of W6+-O and W6+=O bonds, respectively. The electrochemical and optical properties of WO3-x thin films were measured by cyclic voltammetry and UV/vis spectrometry. The results showed the highest charge density at an oxygen flow ratio of 0.7 and the highest transmittance in the visible range. The maximum coloration efficiency was 30.82 cm2/C at an oxygen flow ratio of 0.7.

Mechanochemical synthesis and intercalation of Ca(II)Fe(III)-layered double hydroxides

NASA Astrophysics Data System (ADS)

Ferencz, Zs.; Szabados, M.; Varga, G.; Csendes, Z.; Kukovecz, Á.; Kónya, Z.; Carlson, S.; Sipos, P.; Pálinkó, I.

2016-01-01

A mechanochemical method (grinding the components without added water - dry grinding, followed by further grinding in the presence of minute amount of water or NaOH solution - wet grinding) was used in this work for the preparation and intercalation of CaFe-layered double hydroxides (LDHs). Both the pristine LDHs and the amino acid anion (cystinate and tyrosinate) intercalated varieties were prepared by the two-step grinding procedure in a mixer mill. By systematically changing the conditions of the preparation method, a set of parameters could be determined, which led to the formation of close to phase-pure LDH. The optimisation procedure was also applied for the intercalation processes of the amino acid anions. The resulting materials were structurally characterised by a range of methods (X-ray diffractometry, scanning electron microscopy, energy dispersive analysis, thermogravimetry, X-ray absorption and infra-red spectroscopies). It was proven that this simple mechanochemical procedure was able to produce complex organic-inorganic nanocomposites: LDHs intercalated with amino acid anions.

Solid-State Characterization of Novel Propylene Glycol Ester Solvates Isolated from Lipid Formulations.

PubMed

Chakravarty, Paroma; Kothari, Sanjeev; Deese, Alan; Lubach, Joseph W

2015-07-06

The purpose of this study was to identify and characterize precipitates obtained from a liquid formulation of GNE068.HCl, a Genentech developmental compound, and lipophilic excipients, such as propylene glycol monocaprylate, and monolaurate. Precipitates were characterized using powder X-ray diffractometry (PXRD), differential scanning calorimetry, thermogravimetry, microscopy, nuclear magnetic resonance spectroscopy (NMR; solution and solid-state) and water sorption analysis. PXRD and NMR revealed the precipitates to be crystalline solvates of propylene glycol esters. The solvates (capryolate and lauroglycolate) were isomorphic and stable up to 70 °C, beyond which melting of the lattice occurred with subsequent dissolution of the active ingredient in the melt (microscopy and variable temperature PXRD). They were found to be mechanically stable (no change in PXRD pattern upon compression) and were nonhygroscopic up to ∼70% RH (25 °C). Our results highlight the outcome of inadvertent drug-excipient interactions in two separate lipid solution formulations with good solid-state properties and, thus, potential for further development.

Triphenyltin derivatives of sulfanylcarboxylic esters.

PubMed

Casas, José S; Couce, María D; Sánchez, Agustín; Seoane, Rafael; Sordo, José; Perez-Estévez, Antonio; Vázquez-López, Ezequiel

2018-03-01

The reaction of 3-(aryl)-2-sulfanylpropenoic acids [H 2 xspa; x: p=3-phenyl-, f=3-(2-furyl)-, t=3-(2-thienyl)-] with methanol or ethanol gave the corresponding methyl (Hxspme) or ethyl (Hxspee) esters. The reaction of these esters (HL) with triphenyltin(IV) hydroxide gave compounds of the type [SnPh 3 L], which were isolated and characterized as solids by elemental analysis, IR spectroscopy and mass spectrometry and in solution by multinuclear ( 1 H, 13 C and 119 Sn) NMR spectroscopy. The structures of [SnPh 3 (pspme)], [SnPh 3 (fspme)] and [SnPh 3 (fspee)] were determined by X-ray diffractometry and the antimicrobial activity against E. coli, S. aureus, B. subtilis, P. aeruginosa, Resistant P. aeruginosa (a strain resistant to 'carbapenem'), and C. albicans was tested and the in vitro cytotoxic activity against the HeLa-229, A2780 and A2780cis cell lines was determined for all compounds. Copyright © 2017 Elsevier Inc. All rights reserved.

Preparation of CMC-modified melamine resin spherical nano-phase change energy storage materials.

PubMed

Hu, Xiaofeng; Huang, Zhanhua; Zhang, Yanhua

2014-01-30

A novel carboxymethyl cellulose (CMC)-modified melamine-formaldehyde (MF) phase change capsule with excellent encapsulation was prepared by in situ polymerization. Effects of CMC on the properties of the capsules were studied by Fourier transformation infrared spectroscopy (FTIR), differential scanning calorimetry (DSC), scanning electronic microscopy (SEM), X-ray diffractometry (XRD), and thermogravimetric analysis (TGA). The results showed that the CMC-modified capsules had an average diameter of about 50nm and good uniformity. The phase change enthalpy of the capsules was increased and the cracking ratio decreased by incorporating a suitable amount of CMC. The optimum phase change enthalpy of the nanocapsules was 83.46J/g, and their paraffin content was 63.1%. The heat resistance of the capsule shells decreased after CMC modification. In addition, the nanocapsule cracking ratio of the nanocapsules was 11.0%, which is highly attractive for their application as nano phase change materials. Copyright © 2013 Elsevier Ltd. All rights reserved.

Purification Procedures for Single-Wall Carbon Nanotubes

NASA Technical Reports Server (NTRS)

Gorelik, Olga P.; Nikolaev, Pavel; Arepalli, Sivaram

2001-01-01

This report summarizes the comparison of a variety of procedures used to purify carbon nanotubes. Carbon nanotube material is produced by the arc process and laser oven process. Most of the procedures are tested using laser-grown, single-wall nanotube (SWNT) material. The material is characterized at each step of the purification procedures by using different techniques including scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), transmission electron microscopy (TEM), Raman, X-ray diffractometry (XRD), thermogravimetric analysis (TGA), nuclear magnetic resonance (NMR), and high-performance liquid chromatography (HPLC). The identified impurities are amorphous and graphitic carbon, catalyst particle aggregates, fullerenes, and hydrocarbons. Solvent extraction and low-temperature annealing are used to reduce the amount of volatile hydrocarbons and dissolve fullerenes. Metal catalysts and amorphous as well as graphitic carbon are oxidized by reflux in acids including HCl, HNO3 and HF and other oxidizers such as H2O2. High-temperature annealing in vacuum and in inert atmosphere helps to improve the quality of SWNTs by increasing crystallinity and reducing intercalation.

Synthesization, Characterization, and in Vitro Evaluation of Cytotoxicity of Biomaterials Based on Halloysite Nanotubes.

PubMed

Sánchez-Fernández, Antonio; Peña-Parás, Laura; Vidaltamayo, Román; Cué-Sampedro, Rodrigo; Mendoza-Martínez, Ana; Zomosa-Signoret, Viviana C; Rivas-Estilla, Ana M; Riojas, Paulina

2014-12-04

Halloysite is an aluminosilicate clay that has been widely used for controlled drug delivery, immobilization of enzymes, and for the capture of circulating tumor cells (CTCs). Surface modification of halloysite by organosilanes has been explored to improve their properties. In this study halloysite clay nanotubes (HNTs) were functionalized by two different organosilanes: Trimethoxy(propyl)silane (TMPS), and Triethoxy(octyl)silane (EOS). Untreated and modified samples were characterized by scanning electron microscopy (SEM), X-ray diffractometry (XRD), thermogravimetrical analysis (TGA), and Fourier transform infrared spectroscopy (FTIR). Results showed a strong interaction of organosilanes with the chemical groups present in HNTs. Biocompatibility and cytotoxicity of these nanomaterials were determined using C6 rat glioblastoma cells. Our results indicate that prior to functionalization, HNTs show a high biocompatibility and low cytotoxicity. However, HNTs functionalized with EOS and TMPS showed high cytotoxicity by inducing apoptosis. These results allow the identification of potential applications in biomedical areas for HNTs.

Synthesization, Characterization, and in Vitro Evaluation of Cytotoxicity of Biomaterials Based on Halloysite Nanotubes

PubMed Central

Sánchez-Fernández, Antonio; Peña-Parás, Laura; Vidaltamayo, Román; Cué-Sampedro, Rodrigo; Mendoza-Martínez, Ana; Zomosa-Signoret, Viviana C.; Rivas-Estilla, Ana M.; Riojas, Paulina

2014-01-01

Halloysite is an aluminosilicate clay that has been widely used for controlled drug delivery, immobilization of enzymes, and for the capture of circulating tumor cells (CTCs). Surface modification of halloysite by organosilanes has been explored to improve their properties. In this study halloysite clay nanotubes (HNTs) were functionalized by two different organosilanes: Trimethoxy(propyl)silane (TMPS), and Triethoxy(octyl)silane (EOS). Untreated and modified samples were characterized by scanning electron microscopy (SEM), X-ray diffractometry (XRD), thermogravimetrical analysis (TGA), and Fourier transform infrared spectroscopy (FTIR). Results showed a strong interaction of organosilanes with the chemical groups present in HNTs. Biocompatibility and cytotoxicity of these nanomaterials were determined using C6 rat glioblastoma cells. Our results indicate that prior to functionalization, HNTs show a high biocompatibility and low cytotoxicity. However, HNTs functionalized with EOS and TMPS showed high cytotoxicity by inducing apoptosis. These results allow the identification of potential applications in biomedical areas for HNTs. PMID:28788274

RF sputtered silicon and hafnium nitrides as applied to 440C steel

NASA Technical Reports Server (NTRS)

Grill, A.; Aron, P. R.

1984-01-01

Silicon nitride and hafnium nitride coatings were deposited on oxidized and unoxidized 440C stainless steel substrates. Sputtering was done in mixtures of argon and nitrogen gases from pressed powder silicon nitride and from hafnium metal targets. The coatings and the interface between the coating and substrate were investigated by X-ray diffractometry, scanning electron microscopy, energy dispersive X-ray analysis and Auger electron spectroscopy. Oxide was found at all interfaces with an interface width of at least 600 A for the oxidized substrates and at least 300 A for the unoxidized substrates. Scratch test results demonstrate that the adhesion of hafnium nitride to both oxidized and unoxidized 440C is superior to that of silicon nitride. Oxidized 440C is found to have increased adhesion, to both nitrides, over that of unoxidized 440C. Coatings of both nitrides deposited at 8 mtorr were found to have increased adhesion to both oxidized and unoxidized 440C over those deposited at 20 mtorr.

Mineralogical and Geochemical Analysis of Howardite DaG 779: understanding geological evolution of asteroid (4) Vesta

NASA Astrophysics Data System (ADS)

Marcel Müller, Christian; Mengel, Kurt; Singh Thangjam, Guneshwar; Weckwerth, Gerd

2016-04-01

The HED meteorites, a clan of stony achondrites, are believed to originate from asteroid (4) Vesta (e.g. Mittlefehldt et al. (2015)). Recent evolution models (e.g. Toplis et al. (2013)) and observations from Dawn spacecraft data (e.g., Prettyman et al. (2013)) indicate that diogenites form the lower crust and uppermost mantle of (4) Vesta. Deep seated material excavated by large impacts such as the Rheasilvia- and Veneneiaforming event should be present in howardites. We analysed a slice of howardite DaG 779 which had been recovered from the Libyan Desert in 1999 and was briefly described by Grossmann (2000). The data presented here include electron microprobe, bulk-rock XRD and XRF as well as trace element analysis by ICP-MS and INA. The petrographic results confirm earlier observations that DaG 779 is polymict and mainly contains diogenite and eucrite clasts. Mass balance calculations using bulk-rock and microprobe major element data reveal a modal mineralogy of 77% orthopyroxene, 8% plagioclase, 7% clinopyroxene and 2% spinels, the rest being olivine, SiO2-phases, sulphides, and native Fe(Ni). When compared with the element compilation recently reported by Mittlefehldt (2015) the 39 trace element analysed here (including REE and PGE) confirm that this howardite is clearly dominated by diogenite. Beside the modal petrographic information, a number of more detailed observations obtained from microprobe investigations reveal fresh and recrystallized glasses, troilite-orthopyroxene symplectites from a mixed silicate-sulphide melt giving rise to graphic intergrowths as well as vermicular and reticular FeS in highly disrupted clasts. While the origin of the FeS in these clasts is not clear yet, its particular shape and distribution indicates that this mineral has been (partially) molten and recrystallized from a sulphide melt. The silicate minerals around these FeS occurrences are recrystallized but there is no indication for a partial silicate melt. Further metasomatic reactions were observed between clinopyroxene (pigeonite) and a sulphide-bearing agent, according to the principal reaction Pigeonite (Fe-rich) + S2 ↔ FeS + Augit (Mg-rich) + SiO2. This type of metasomatism (Zhang et al. (2013)) is not well understood yet. References: Grossman, J. N. (2000): The Meteoritical Bulletin, No. 84, 2000 August. Meteoritics & Planetary Science, 35: A119-A225. doi: 10.1111/j.1945-5100.2000.tb01797.x. Toplis, M.J. et al. (2013): Chondritic models of 4 Vesta: Implications for geochemical and geophysical properties. Meteoritics & Planetary Science, 48: 2300-2315. doi: 10.1111/maps.12195. Zhang, A. et al. (2013): Record of S-rich vapors on asteroid 4 Vesta: Sulfurization in the Northwest Africa 2339 eucrite. Geochim. Cosmochim. Acta 109, 1-13. Mittlefehldt, D.W., (2015): Asteroid (4) Vesta: I. The howardite-eucrite-diogenite (HED) clan of meteorites. Chemie Erde-Geochem. 75, 2, 155-183. Prettyman, T.H. et al. (2013): Neutron absorption constraints on the composition of 4 Vesta. Meteoritics & Planetary Science 48:2211-2236.

Changes in seasonal climate patterns from 34-4 ka in a Soreq Cave (Israel) speleothem: Sub-annual resolution by ion microprobe and CLFM

NASA Astrophysics Data System (ADS)

Orland, I. J.; Bar-Matthews, M.; Kita, N.; Ayalon, A.; Valley, J. W.

2009-12-01

Speleothems provide an important proxy-record of paleoclimate. Isotopic data from calcite-dominated cave formations have been used to identify changes in annual rainfall, monsoon strength, telecommunication of Northern Hemisphere climate aberrations, changes in vegetation cover, and other region-specific paleoclimate time-series over annual to millennial timescales. As more research is devoted to understanding abrupt climate change events, there is a need to develop high-temporal-resolution records from continental regions. However, in most isotopic studies, seasonality information is lost due to technical limitations. This study focuses on a speleothem from the semi-arid Eastern Mediterranean region (Soreq Cave, Israel) where prior research shows that conventional drill-sampling methods permit a temporal resolution of ~10-50 years in speleothem paleoclimate records. The WiscSIMS lab has developed analytical protocols for ion microprobe analysis that yield a precision of ~0.3‰ (2 s.d.) in δ18O from 10 μm-diameter spots, which permit multiple analyses/year in many speleothems. Orland et al. (2009, Quat. Res.) establish the methodology for the current study by identifying seasonal variability using a combination of confocal laser fluorescent microscopy (CLFM) and ion microprobe analysis in a younger (~2-1 ka) Soreq speleothem that has a consistent bright-grading-to-dark fluorescence pattern within each annual band. Further, Orland et al. define a quantitative measure of seasonality, Δ18O, that measures the difference in δ18O between bright and dark fluorescent portions of individual annual growth bands [Δ18O = δ18Odark - δ18Obright]. Smaller values of Δ18O are interpreted to be caused by dry years. The current study employs the aforementioned methods to examine seasonality trends in a sample that covers a much longer time period. We report δ18O from >1000 spots across a radial traverse of Soreq Cave sample 2N matched to imaging of annual growth bands by CLFM. This record, which extends from 34-4 ka, based on 27 new U-Th dates from the Geological Survey of Israel, preserves a time-series of δ18O across multiple significant climate changes including the last glacial termination, the onset/termination of the YD, and multiple abrupt regional events. As in the younger sample from Soreq, CLFM of the Holocene portion of sample 2N reveals concentric, annual growth bands in bright-grading-to-dark fluorescent couplets. In the pre-Holocene portion of 2N, however, the pattern of fluorescence banding is consistently reversed (i.e. dark-grading-to-bright). Furthermore, the magnitude of Δ18O changes through time. The prominent change in the CLFM and Δ18O record for sample 2N suggests a shift in seasonality in the Eastern Mediterranean before the termination of the YD; variation in seasonal rainfall and/or surface vegetation may have contributed to the observed change.

Raman mapping of mannitol/lysozyme particles produced via spray drying and single droplet drying.

PubMed

Pajander, Jari Pekka; Matero, Sanni; Sloth, Jakob; Wan, Feng; Rantanen, Jukka; Yang, Mingshi

2015-06-01

This study aimed to investigate the effect of a model protein on the solid state of a commonly used bulk agent in spray-dried formulations. A series of lysozyme/mannitol formulations were spray-dried using a lab-scale spray dryer. Further, the surface temperature of drying droplet/particles was monitored using the DRYING KINETICS ANALYZER™ (DKA) with controllable drying conditions mimicking the spray-drying process to estimate the drying kinetics of the lysozyme/mannitol formulations. The mannitol polymorphism and the spatial distribution of lysozyme in the particles were examined using X-ray powder diffractometry (XRPD) and Raman microscopy. Partial Least Squares Discriminant Analysis was used for analyzing the Raman microscopy data. XRPD results indicated that a mixture of β-mannitol and α-mannitol was produced in the spray-drying process which was supported by the Raman analysis, whereas Raman analysis indicated that a mixture of α-mannitol and δ-mannitol was detected in the single particles from DKA. In addition Raman mapping indicated that the presence of lysozyme seemed to favor the appearance of α-mannitol in the particles from DKA evidenced by close proximity of lysozyme and mannitol in the particles. It suggested that the presence of lysozyme tend to induce metastable solid state forms upon the drying process.

Organic-Inorganic Hydrophobic Nanocomposite Film with a Core-Shell Structure

PubMed Central

Liu, Peng; Chen, Ying; Yu, Zhiwu

2016-01-01

A method to prepare novel organic-inorganic hydrophobic nanocomposite films was proposed by a site-specific polymerization process. The inorganic part, the core of the nanocomposite, is a ternary SiO2–Al2O3–TiO2 nanoparticles, which is grafted with methacryloxy propyl trimethoxyl silane (KH570), and wrapped by fluoride and siloxane polymers. The synthesized samples are characterized by transmission electron microscopy (TEM), Fourier transform infrared (FTIR) spectrscopy, X-ray diffractometry (XRD), contact angle meter (CA), and scanning electron microscope (SEM). The results indicate that the novel organic-inorganic hydrophobic nanocomposite with a core-shell structure was synthesized successfully. XRD analysis reveals the nanocomposite film has an amorphous structure, and FTIR analysis indicates the nanoparticles react with a silane coupling agent (methacryloxy propyl trimethoxyl silane KH570). Interestingly, the morphology of the nanoparticle film is influenced by the composition of the core. Further, comparing with the film synthesized by silica nanoparticles, the film formed from SiO2–Al2O3–TiO2 nanoparticles has higher hydrophobic performance, i.e., the contact angle is greater than 101.7°. In addition, the TEM analysis reveals that the crystal structure of the particles can be changed at high temperatures. PMID:28774141

Thermal events documented in Hadean zircons by ion microprobe depth profiles

NASA Astrophysics Data System (ADS)

Trail, Dustin; Mojzsis, Stephen J.; Harrison, T. Mark

2007-08-01

We report the first U-Th-Pb ion microprobe depth profiles of four Hadean zircons from the Jack Hills and Mount Narryer supracrustal belts of the Narryer Gneiss Complex (NGC), Western Australia. This ultra-high spatial resolution technique probes the age and origin of sub-micron features in individual crystals that can record episodes of zircon growth. Near-surface grain dates of 2700 Ma or older are coincident with post-depositional growth/modification. Some ages may coincide with documented pre-deposition metamorphic events for the NGC and igneous emplacement at ca. 3700 Ma. Separate events that do not correlate in time with known geologic episodes prior to the preserved rock record are also present on pre-4000 Ma zircons. We find evidence for a ˜3.9 Ga event, which is coterminous within age uncertainty with one or several large basin-forming impacts (e.g. Nectaris) on the Moon attributed to the late heavy bombardment of the inner solar system.

Ion microprobe analyses of aluminous lunar glasses - A test of the 'rock type' hypothesis

NASA Technical Reports Server (NTRS)

Meyer, C., Jr.

1978-01-01

Previous soil survey investigations found that there are natural groupings of glass compositions in lunar soils and that the average major element composition of some of these groupings is the same at widely separated lunar landing sites. This led soil survey enthusiasts to promote the hypothesis that the average composition of glass groupings represents the composition of primary lunar 'rock types'. In this investigation the trace element composition of numerous aluminous glass particles was determined by the ion microprobe method as a test of the above mentioned 'rock type' hypothesis. It was found that within any grouping of aluminous lunar glasses by major element content, there is considerable scatter in the refractory trace element content. In addition, aluminous glasses grouped by major elements were found to have different average trace element contents at different sites (Apollo 15, 16 and Luna 20). This evidence argues that natural groupings in glass compositions are determined by regolith processes and may not represent the composition of primary lunar 'rock types'.

SXRF determination of trace elements in chondrule rims in the unequilibrated CO3 chondrite, ALH A77307

NASA Technical Reports Server (NTRS)

Brearley, Adrian J.; Bajt, Sasa; Sutton, Steve R.; Papike, J. J.

1993-01-01

The concentrations of Ni, Cu, Zn, Ga, Ge, and Se in five chondrule rims in the CO3 chondrite ALH A77307 (3.0) using the synchrotron x-ray fluorescence (SXRF) microprobe at Brookhaven National Laboratory were determined. The data show that the trace element chemistry of rims on different chondrules is remarkably similar, consistent with data obtained for the major elements by electron microprobe. These results support the idea that rims are not genetically related to individual chondrules, but all sampled the same reservoir of homogeneously mixed dust. Of the trace elements analyzed Zn and Ga show depletions relative to CI chondrite values, but in comparison with bulk CO chondrites all the elements are enriched by approximately 1.5 to 3.5 x CO. The high concentrations of the highly volatile elements Se and Ga and moderately volatile Zn (1.5 to 2 x CO) in rims show that matrix is the major reservoir of volatile elements in ALH A77307.

KSC-98pc1627

NASA Image and Video Library

1998-11-10

KENNEDY SPACE CENTER, FLA. -- In the Spacecraft Assembly and Encapsulation Facility -2 (SAEF-2), Chris Voorhees and Satish Krishnan from the Jet Propulsion Laboratory remove a microprobe which will hitchhike on the Mars Polar Lander. Scheduled to be launched Jan. 3, 1999, aboard a Delta II rocket, the solar-powered spacecraft is designed to touch down on the Martian surface near the northern-most boundary of the south pole in order to study the water cycle there. The lander also will help scientists learn more about climate change and current resources on Mars, studying such things as frost, dust, water vapor and condensates in the Martian atmosphere. The Mars microprobes, called Deep Space 2, are part of NASA's New Millennium Program. They will complement the climate-related scientific focus of the lander by demonstrating an advanced, rugged microlaser system for detecting subsurface water. Such data on polar subsurface water, in the form of ice, should help put limits on scientific projections for the global abundance of water on Mars

Rare Earth elements in individual minerals in Shergottites

NASA Technical Reports Server (NTRS)

Wadhwa, Meenakshi; Crozaz, Ghislaine

1993-01-01

Shergottites (i.e., Shergotty, Zagami, EETA79001, ALHA77005, and LEW88516) are an important set of achondrites because they comprise the majority of the SNC group of meteorites (nine, in total, known to us), which are likely to be samples of the planet Mars. Study of these meteorites may therefore provide valuable information about petrogenetic processes on a large planetary body other than Earth. Rare earth element (REE) distributions between various mineral phases were found to be useful in geochemically modeling the petrogenesis of various rock types (terrestrial and meteoritic). However, with the exception of a few ion microprobe studies and analyses of mineral separates, there has previously not been any comprehensive effort to characterize and directly compare REE in individual minerals in each of the five known shergottites. Ion microprobe analyses were made on thin sections of each of the shergottites. Minerals analyzed were pyroxenes (pigeonite and augite), maskelynite, and whitlockite. The REE concentrations in each mineral type in each shergottite is given.

Differential phase contrast with a segmented detector in a scanning X-ray microprobe

PubMed Central

Hornberger, B.; de Jonge, M. D.; Feser, M.; Holl, P.; Holzner, C.; Jacobsen, C.; Legnini, D.; Paterson, D.; Rehak, P.; Strüder, L.; Vogt, S.

2008-01-01

Scanning X-ray microprobes are unique tools for the nanoscale investigation of specimens from the life, environmental, materials and other fields of sciences. Typically they utilize absorption and fluorescence as contrast mechanisms. Phase contrast is a complementary technique that can provide strong contrast with reduced radiation dose for weakly absorbing structures in the multi-keV range. In this paper the development of a segmented charge-integrating silicon detector which provides simultaneous absorption and differential phase contrast is reported. The detector can be used together with a fluorescence detector for the simultaneous acquisition of transmission and fluorescence data. It can be used over a wide range of photon energies, photon rates and exposure times at third-generation synchrotron radiation sources, and is currently operating at two beamlines at the Advanced Photon Source. Images obtained at around 2 keV and 10 keV demonstrate the superiority of phase contrast over absorption for specimens composed of light elements. PMID:18552427

Modified extrusion-spheronization as a technique of microencapsulation for stabilization of choline bitartrate using hydrogenated soya bean oil.

PubMed

Gangurde, Avinash Bhaskar; Sav, Ajay Kumar; Javeer, Sharadchandra Dagadu; Moravkar, Kailas K; Pawar, Jaywant N; Amin, Purnima D

2015-01-01

Choline bitartrate (CBT) is a vital nutrient for fetal brain development and memory function. It is hygroscopic in nature which is associated with stability related problem during storage such as development of fishy odor and discoloration. Microencapsulation method was adopted to resolve the stability problem and for this hydrogenated soya bean oil (HSO) was used as encapsulating agent. Industrially feasible modified extrusion-spheronization technique was selected for microencapsulation. HSO was used as encapsulating agent, hydroxypropyl methyl cellulose E5/E15 as binder and microcrystalline cellulose as spheronization aid. Formulated pellets were evaluated for parameters such as flow property, morphological characteristics, hardness-friability index (HFI), drug content, encapsulation efficiency, and in vitro drug release. The optimized formulations were also characterized for particle size (by laser diffractometry), differential scanning calorimetry, powder X-ray diffractometry (PXRD), Fourier transform infrared spectroscopy, and scanning electron microscopy. The results from the study showed that coating of 90% and 60% CBT was successful with respect to all desired evaluation parameters. Optimized formulation was kept for 6 months stability study as per ICH guidelines, and there was no change in color, moisture content, drug content, and no fishy odor was observed. Microencapsulated pellets of CBT using HSO as encapsulating agent were developed using modified extrusion spheronization technique. Optimized formulations, CBT 90% (F5), and CBT 60% (F10), were found to be stable for 4M and 6M, respectively, at accelerated conditions.

Application of film-casting technique to investigate drug-polymer miscibility in solid dispersion and hot-melt extrudate.

PubMed

Parikh, Tapan; Gupta, Simerdeep Singh; Meena, Anuprabha K; Vitez, Imre; Mahajan, Nidhi; Serajuddin, Abu T M

2015-07-01

Determination of drug-polymer miscibility is critical for successful development of solid dispersions. This report details a practical method to predict miscibility and physical stability of drug with various polymers in solid dispersion and, especially, in melt extrudates by applying a film-casting technique. Mixtures of itraconazole (ITZ) with hydroxypropylmethylcellulose phthalate (HPMCP), Kollidon(®) VA 64, Eudragit(®) E PO, and Soluplus(®) were film-casted, exposed to 40°C/75% RH for 1 month and then analyzed using differential scanning calorimetry (DSC), powder X-ray diffractometry, and polarized light microscopy (PLM). ITZ had the highest miscibility with HPMCP, being miscible at drug to polymer ratio of 6:4 (w/w). There was a downward trend of lower miscibility with Soluplus(®) (miscible at 3:7, w/w, and a few microcrystals present at 4:6, w/w), Kollidon(®) VA 64 (2:8, w/w) and Eudragit(®) E PO (<1:9, w/w). PLM was found more sensitive to detect drug crystallization than DSC and powder X-ray diffractometry. There was general correlation between results of film casting and hot-melt extrusion (HME) using a twin screw extruder. For ITZ-Soluplus(®) mixtures, HME at 4:6 (w/w) resulted in a single phase, whereas drug crystallization was observed at higher drug load. HME of ITZ-Kollidon(®) VA 64 mixtures also correlated well with the miscibility predicted by film casting. © 2015 Wiley Periodicals, Inc. and the American Pharmacists Association.

The Systematics of Light Lithophile Elements (Li, Be, B) in Lunar Picritic Glasses

NASA Astrophysics Data System (ADS)

Shearer, C. K.; Layne, G. D.; Papike, J. J.

1993-07-01

Lunar picritic glasses are thought to be the product of either partial melting of the deep lunar mantle followed by rapid ascent [1,2] or polybaric partial melting initiated in the deep lunar mantle [3]. The near primary compositions of these volcanic glasses provide us with a unique perspective for evaluating mare basaltic magmatism and the characteristics and evolution of the lunar mantle. Because of their obvious importance in deciphering the evolution of the Earth-Moon system, we have initiated an extensive trace element study of these picritic glasses using ion microprobe techniques. Here, we report the initial results of light lithophile element (LLE) analyses of these glasses. This is the first reported study of LLE in lunar basalts. The LLE have only recently received attention in terrestrial basaltic systems [4-6]. Their correlations with other more routinely analyzed trace elements (Li:Yb or V, Be:Nd, B:K) in a variety of terrestrial mantle environments have yielded several important insights into mantle magmatism [4-6]. Ion microprobe analyses of the glasses were conducted using a Cameca 4f ion microprobe operated on the UNM campus. The light lithophile elements were analyzed under the following conditions: 10-kV O- primary beam, 8-nA primary beam current, 10-15-micrometer beam diameter, sample voltage offset of -70 +- 25 V, and a 150-micrometer secondary ion image field with a 33-micrometer field aperature inserted. Counting times included background (2 seconds), 30Si (2 seconds), 7Li (2 seconds), 9Be (4 seconds), and 11B (8 seconds). Each analysis involved 30 to 40 counting cycles. These counting times resulted in precision for Li of better than 1.2% and for B and Be of better than 2.2%. Standards for Li, Be, and B in basaltic glass matrices were kindly provided by J. Ryan [4-6]. Calibration curves (LLE/30Si x wt% SiO2 vs. LLE concentration) were originally defined by a minimum of five standards for each element and are linear for the concentration ranges found in the picritic lunar glasses. Picritic glasses analyzed in the initial study were from the Apollo 12, 14, 15, and 17 sites. This suite of glasses ranged in TiO2 from 0.3 to 17 wt%. All glasses had been previously analyzed for major and trace elements (REE, Cr, V, Sr, Ba, Co, Zr) by electron microprobe and ion microprobe [2]. The LLE show a wide range of variability with Li ranging from 1.2 to 23.8 ppm, Be ranging from 0.06 to 3.09 ppm, and B ranging from 0.20 to 3.87 ppm. Traverses across individual glass beads suggest they are homogeneous with regard to LLE. Except for the A17 VLT glasses and the A15 yellow glasses, the individual glass groups [1] show very limited LLE variability. LLE content is positively correlated to TiO2 content. LLE concentrations also parallel the enrichment of other lithophile elements such as Ba, Zr, Sr, and the REE. Unlike terrestrial basalts [4-6], the concentration of LLE in the picritic glasses is negatively correlated with SiO2 and MgO. B/Be ranges from 0.40 to 4.6. Over 85% of the analyzed glasses have B/Be between 0.9 and 3.0, similar to the average B/Be value of 3 for MORB [6]. Li/B and Li/Be values range from 3.2 to 30.8 and 2.7 to 41.7, respectively. These LLE ratios are not correlated with TiO2, but appear to be characteristic of individual sampling sites and therefore reflect subtle differences in the sources of the picritic magmas. The LLE and LLE ratios also indicate a KREEP component had been incorporated into some of these picritic magmas. Shearer and Papike [2] suggested this incorporation occurs in the zone of melting and reflected overturning of the LMO cumulate pile. The initial data reported here suggest that the LLE may be useful in deciphering the mare basalt record. Further analyses of these glasses will allow a more detailed comparison of picritic glass sources with mare basalt sources and a better interpretation of the compositional relationships among picritic glasses. Acknowledgments: SIMS analyses were performed at the UNM/SNL Ion Microprobe Facility, a joint operation of the Institute of Meteoritics, UNM, and Sandia National Laboratories. This research was funded by NASA grant NAGW-3347. References: [1] Delano J. W. (1986) Proc. LPSC, 16th, in JGR, XX D201-D213. [2] Shearer C. K. and Papike J. J. (1993) GCA, in review. [3] Longhi J. (1992) GCA, 56, 2235-2252. [4] Ryan J. G. and Langmuir C. H. (1987) GCA, 51, 1727- 1741. [5] Ryan J. G. and Langmuir C. H. (1988) GCA, 52, 237-244. [6] Ryan J. G. and Langmuir C. H. (1993) GCA, 57, 1489-1498.

The solid state of rebamipide: preparation, characterization, and dissolution.

PubMed

Jeon, Seong Hyeon; Sohn, Young Taek

2016-04-01

Rebamipide is marketed as a peptic ulcer agent under the trade name Mucosta(R). The objective of this work was to investigate the existence of polymorphs and pseudopolymorphs of rebamipide. Two crystal forms of rebamipide were isolated by recrystallization and characterized by differential thermal analysis (DTA), thermogravimetric analysis (TG), powder X-ray diffractometry, infrared spectrometry, and nuclear magnetic resonance. The DTA curve of Form 1 showed one endothermic peak at 305.2 °C, and that of Form 2 showed one endothermic peak at 307.3 °C. The TG curve of Form 1 showed a single weight loss at 305.2 °C, which corresponded to melting. The TG curve of Form 2 also showed a single weight loss at 307.3 °C, which corresponded to melting. The melting point of Form 2 was higher than that of Form 1. In the dissolution studies in pH 6.8 buffer at 37 ± 0.5 °C, the two crystal forms showed no significant differences in dissolution. After 3 months of storage at 0, 52, and 95% RH, the two crystal forms were not transformed. After milling with a Specamill for 2 h, the two crystal forms were not transformed.

Synthesis of high generation thermo-sensitive dendrimers for extraction of rivaroxaban from human fluid and pharmaceutic samples.

PubMed

Parham, Negin; Panahi, Homayon Ahmad; Feizbakhsh, Alireza; Moniri, Elham

2018-04-13

In this present study, poly (N-isopropylacrylamide) as a thermo-sensitive agent was grafted onto magnetic nanoparticles, then ethylenediamine and methylmethacrylate were used to synthesize the first generation of poly amidoamine (PAMAM) dendrimers successively and the process continued alternatively until the ten generations of dendrimers. The synthesized nanocomposite was investigated using Fourier transform infrared spectrometry, thermalgravimetry analysis, X-ray diffractometry, elemental analysis and vibrating-sample magnetometer. The particle size and morphology were characterized using dynamic light scattering, field emission scanning electron microscopy and transmission electron microscopy. Batch experiments were conducted to investigate the parameters affecting adsorption and desorption of rivaroxaban by synthesized nanocomposite. The maximum sorption of rivaroxaban by the synthesized nanocomposite was obtained at pH of 8. The resulting grafted magnetic nanoparticle dendrimers were applied for extraction of rivaroxaban from biologic human liquids and medicinal samples. The specifications of rivaroxaban sorbed by a magnetic nanoparticle dendrimer showed good accessibility and high capacity of the active sites within the dendrimers. Urine and drug matrix extraction recoveries of more than 92.5 and 99.8 were obtained, respectively. Copyright © 2018 Elsevier B.V. All rights reserved.

Synthesis and characterization of ferrite-semiconductor nano composite for photocatalytic degradation of aqueous nitrobenzene solution

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

Modi, K. B.; Kathad, C. R.; Raval, P. Y.

2016-05-06

Nanoparticles of semiconductor TiO{sub 2}, zinc ferrite (ZnFe{sub 2}O{sub 4}) and ZnFe{sub 2}O{sub 4}-TiO{sub 2} composite, were synthesized by auto combustion route. Subsequent characterization of synthesized photocatalysts was carried out by X-ray powder diffractometry, transmission electron microscopy, UV-Vis-Diffuse Reflectance Spectroscopy to study the structural and textural properties. The specific surface area, pore diameter and pore volume of synthesized materials were investigated by N{sub 2} adsorption analysis while the presence of TiO{sub 2} in the composite material was verified by infrared spectral analysis. The photocatalytic activity of synthesized photocatalysts was evaluated by degradation of nitrobenzene (NB) in aqueous medium under irradiationmore » of ultraviolet light. The result revealed that 77, 73 and 70% of NB was degraded using TiO{sub 2}, ZnFe{sub 2}O{sub 4} and ZnFe{sub 2}O{sub 4}-TiO{sub 2} photocatalysts after 4h in the presence of UV irradiation. The composite photocatalyst was found easy to separate from the treated solution.« less

Investigations on nucleation, HRXRD, optical, piezoelectric, polarizability and Z-scan analysis of L-arginine maleate dihydrate single crystals

NASA Astrophysics Data System (ADS)

Sakthy Priya, S.; Alexandar, A.; Surendran, P.; Lakshmanan, A.; Rameshkumar, P.; Sagayaraj, P.

2017-04-01

An efficient organic nonlinear optical single crystal of L-arginine maleate dihydrate (LAMD) has been grown by slow evaporation solution technique (SEST) and slow cooling technique (SCT). The crystalline perfection of the crystal was examined using high-resolution X-ray diffractometry (HRXRD) analysis. Photoluminescence study confirmed the optical properties and defects level in the crystal lattice. Electromechanical behaviour was observed using piezoelectric co-efficient (d33) analysis. The photoconductivity analysis confirmed the negative photoconducting nature of the material. The dielectric constant and loss were measured as a function of frequency with varying temperature and vice-versa. The laser damage threshold (LDT) measurement was carried out using Nd:YAG Laser with a wavelength of 1064 nm (Focal length is 35 cm) and the obtained results showed that LDT value of the crystal is high compared to KDP crystal. The high laser damage threshold of the grown crystal makes it a potential candidate for second and higher order nonlinear optical device application. The third order nonlinear optical parameters of LAMD crystal is determined by open-aperture and closed-aperture studies using Z-scan technique. The third order linear and nonlinear optical parameters such as the nonlinear refractive index (n2), two photon absorption coefficient (β), Real part (Reχ3) and imaginary part (Imχ3) of third-order nonlinear optical susceptibility are calculated.

Nickel and cobalt distribution in the laterites of the Lomié region, south-east Cameroon

NASA Astrophysics Data System (ADS)

Yongue-Fouateu, R.; Ghogomu, R. T.; Penaye, J.; Ekodeck, G. E.; Stendal, H.; Colin, F.

2006-05-01

In the Lomié region (south-east Cameroon), strong weathering of serpentinized ultramafic rocks has produced a thick laterite cover with significant nickel and cobalt contents. The highest concentrations of these elements are located in the middle section of the laterite profiles, in the lower clay horizon, and preferentially along the slopes of the interfluves. The investigation of the composition of the laterite ores (by whole-rock analysis) and of the main components, using SEM/microprobe and XRD, reveals the presence of four main enriched facies: a non-differentiated facies, a layered smectitic facies, a quartz-rich facies and a gibbsitic nodular facies. Nickel, with generally low concentrations (less than 2% NiO), is hosted by several secondary mineral phases (goethite, Mn-oxyhydroxides and smectite locally). Cobalt is generally of higher grade (up to 0.9% CoO), and is associated with cryptocrystalline and crystallized Mn-oxyhydroxides. SEM/microprobe observations suggest that nickel and cobalt concentration in secondary minerals is due to repeated remobilization. This has also favored the formation of mineral phases, of which the best crystallized and most richly mineralized are mainly those of the asbolan-lithiophorite group. The SEM studies indicate that these mineral phases show various morphologies related to their chemical composition: poorly crystallized nipple shaped (Fe, Mn, Ni), fine cross-bedded needles (Mn, Ni) and elongated crystals (Mn, Al, Ni, Co) occur in the layered smectitic facies, while platy and needle-like forms (Mn, Al, Ni, Co) characterize the gibbsitic nodular facies. The predominantly cobaltiferous nature of the Lomié laterite ore deposit is the result of remobilizations and transformations of elements that led to the impoverishment of both the Ni-Co contents of the laterite but most importantly of Ni rather than Co.

238U-230Th dating of chevkinite in high-silica rhyolites from La Primavera and Yellowstone calderas

USGS Publications Warehouse

Vazquez, Jorge A.; Velasco, Noel O.; Schmitt, Axel K.; Bleick, Heather A.; Stelten, Mark E.

2014-01-01

Application of 238U-230Th disequilibrium dating of accessory minerals with contrasting stabilities and compositions can provide a unique perspective on magmatic evolution by placing the thermochemical evolution of magma within the framework of absolute time. Chevkinite, a Th-rich accessory mineral that occurs in peralkaline and metaluminous rhyolites, may be particularly useful as a chronometer of crystallization and differentiation because its composition may reflect the chemical changes of its host melt. Ion microprobe 128U-230Th dating of single chevkinite microphenocrysts from pre- and post-caldera La Primavera, Mexico, rhyolites yields model crystallization ages that are within 10's of k.y. of their corresponding K-Ar ages of ca. 125 ka to 85 ka, while chevkinite microphenocrysts from a post-caldera Yellowstone, USA, rhyolite yield a range of ages from ca. 110 ka to 250 ka, which is indistinguishable from the age distribution of coexisting zircon. Internal chevkinite-zircon isochrons from La Primavera yield Pleistocene ages with ~5% precision due to the nearly two order difference in Th/U between both minerals. Coupling chevkinite 238U-230Th ages and compositional analyses reveals a secular trend of Th/U and rare earth elements recorded in Yellowstone rhyolite, likely reflecting progressive compositional evolution of host magma. The relatively short timescale between chevkinite-zircon crystallization and eruption suggests that crystal-poor rhyolites at La Primavera were erupted shortly after differentiation and/or reheating. These results indicate that 238U-230Th dating of chevkinite via ion microprobe analysis may be used to date crystallization and chemical evolution of silicic magmas.

Isotopic Measurements in CAIs with the Nanosims: Implications to the understanding of the Formation process of Ca, Al-Rich Inclusions

NASA Technical Reports Server (NTRS)

Ito, M.; Messenger, S.; Walker, Robert M.

2007-01-01

Ca, Al-rich Inclusions (CAIs) preserve evidence of thermal events that they experienced during their formation in the early solar system. Most CAIs from CV and CO chondrites are characterized by large variations in O-isotopic compositions of primary minerals, with spinel, hibonite, and pyroxene being more O-16-rich than melilite and anorthite, with delta 17, O-18 = approx. -40%o (DELTA O-17 = delta O-17 - 0.52 x delta O-18 = approx. - 20%o ). These anomalous compositions cannot be accounted for by standard mass dependent fractionation and diffusive process of those minerals. It requires the presence of an anomalous oxygen reservoir of nucleosynthetic origin or mass independent fractionations before the formation of CAIs in the early solar system. The CAMECA NanoSIMS is a new generation ion microprobe that offers high sensitivity isotopic measurements with sub 100 nm spatial resolution. The NanoSIMS has significantly improved abilities in the study of presolar grains in various kind of meteorites and the decay products of extinct nuclides in ancient solar system matter. This instrument promises significant improvements over other conventional ion probes in the precision isotopic characterization of sub-micron scales. We report the results of our first O isotopic measurements of various CAI minerals from EK1-6-3 and 7R19-1(a) utilizing the JSC NanoSIMS 50L ion microprobe. We evaluate the measurement conditions, the instrumental mass fractionation factor (IMF) for O isotopic measurement and the accuracy of the isotopic ratio through the analysis of a San Carlos olivine standard and CAI sample of 7R19-1(a).

Geochemistry of HASP, VLT, and other glasses from double drive tube 79001/2

NASA Technical Reports Server (NTRS)

Lindstrom, D. J.; Wentworth, S. J.; Martinez, R. R.; Mckay, D. S.

1992-01-01

The Apollo 17 double drive tube 79001/2 (station 9, Van Serg Crater) is distinctive because of its extreme maturity, abundance, and variety of glass clasts. It contains mare glasses of both high Ti and very low Ti (VLT) compositions, and highland glasses of all compositions common in lunar regolith samples: highland basalt (feldspathic; Al2O3 greater than 23 wt percent), KREEP (Al2O3 less than 23 wt percent, K2O greater than 0.25 wt percent), and low-K Fra Mauro (LKFM; Al2O3 less than 23 wt percent, K2O less than 0.25 wt percent). It also contains rare specimens of high-alumina, silica-poor (HASP), and ultra Mg glasses. HASP glasses contain insufficient SiO2 to permit the calculation of a standard norm, and are thought to be the product of volatilization during impact melting. They have been studied by electron microprobe major-element analysis techniques but have not previously been analyzed for trace elements. The samples analyzed for this study were polished grain mounts of the 90-160 micron fraction of four sieved samples from the 79001/2 core (depth range 2.3-11.5 cm). A total of 80 glasses were analyzed by SEM/EDS and electron microprobe, and a subset of 33 of the glasses, representing a wide range of compositional types, was chosen for high-sensitivity INAA. A microdrilling device removed disks (mostly 50-100 micron diameter, weighing approx. 0.1-0.5 micro-g) for INAA. Preliminary data reported here are based only on short counts done within two weeks of irradiation.

CALCMIN - an EXCEL™ Visual Basic application for calculating mineral structural formulae from electron microprobe analyses

NASA Astrophysics Data System (ADS)

Brandelik, Andreas

2009-07-01

CALCMIN, an open source Visual Basic program, was implemented in EXCEL™. The program was primarily developed to support geoscientists in their routine task of calculating structural formulae of minerals on the basis of chemical analysis mainly obtained by electron microprobe (EMP) techniques. Calculation programs for various minerals are already included in the form of sub-routines. These routines are arranged in separate modules containing a minimum of code. The architecture of CALCMIN allows the user to easily develop new calculation routines or modify existing routines with little knowledge of programming techniques. By means of a simple mouse-click, the program automatically generates a rudimentary framework of code using the object model of the Visual Basic Editor (VBE). Within this framework simple commands and functions, which are provided by the program, can be used, for example, to perform various normalization procedures or to output the results of the computations. For the clarity of the code, element symbols are used as variables initialized by the program automatically. CALCMIN does not set any boundaries in complexity of the code used, resulting in a wide range of possible applications. Thus, matrix and optimization methods can be included, for instance, to determine end member contents for subsequent thermodynamic calculations. Diverse input procedures are provided, such as the automated read-in of output files created by the EMP. Furthermore, a subsequent filter routine enables the user to extract specific analyses in order to use them for a corresponding calculation routine. An event-driven, interactive operating mode was selected for easy application of the program. CALCMIN leads the user from the beginning to the end of the calculation process.

Ion and electron microprobe study of troctolites, norite, and anorthosites from Apollo 14: Evidence for urKREEP assimilation during petrogenesis of Apollo 14 Mg-suite rocks

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

Shervais, J.W.; McGee, J.J.

1998-09-01

Most of the Moon`s highland crust comprises Fe-rich anorthosites with calcic plagioclase compositions. Subsequent evolution of the highland crust was dominated by troctolites, anorthosites, and norites of the Mg-suite. This plutonic series is characterized by calcic plagioclase, and mafic minerals with high mg{number_sign} (=100{sup *}Mg/[Mg + Fe]). In an effort to distinguish the origin of this important lunar rock series, the authors have analyzed the REE content of primary cumulus phases in ten Mg-suite cumulates using SIMS, along with their major and minor element compositions by electron microprobe analysis. Nine of these samples have high mg{number_sign}s, consistent with their formationmore » from the most primitive parent melts of the Mg-suite. The data presented here show that Mg-suite troctolites and anorthosites preserve major and trace element characteristics acquired during their formation as igneous cumulate rocks and that these characteristics can be used to reconstruct related aspects of the parent magma composition. Data show that primitive cumulates of the Mg-suite crystallized from magmas with REE contents similar to high-K KREEP in both concentration and relative abundance. The highly enriched nature of this parent magma contrasts with its primitive major element characteristics, as pointed out by previous workers. This enigma is best explained by the mixing of residual magma ocean urKREEP melts with ultramagnesian komatiitic partial melts from the deep lunar interior. The data do not support earlier models that invoke crustal metasomatism to enrich the Mg-suite cumulates after formation, or models which call for a superKREEP parent for the troctolites and anorthosites.« less

Measurements of the quantitative lateral analytical resolution at evaporated aluminium and silver layers with the JEOL JXA-8530F FEG-EPMA

NASA Astrophysics Data System (ADS)

Berger, D.; Nissen, J.

2018-01-01

The studies in this paper are part of systematic investigations of the lateral analytical resolution of the field emission electron microprobe JEOL JXA-8530F. Hereby, the quantitative lateral resolution, which is achieved in practise, is in the focus of interest. The approach is to determine the minimum thickness of a metallic layer for which an accurate quantitative element analysis in cross-section is still possible. Previous measurements were accomplished at sputtered gold (Z = 79) layers, where a lateral resolution in the range of 140 to 170 nm was achieved at suitable parameters of the microprobe. To study the Z-dependence of the lateral resolution, now aluminium (Z = 13) resp. silver (Z = 47) layers with different thicknesses were generated by evaporation and prepared in cross-section subsequently by use of a focussed Ga-ion beam (FIB). Each layer was analysed quantitatively with different electron energies. The thinnest layer which can be resolved specifies the best lateral resolution. These measured values were compared on the one hand with Monte Carlo simulations and on the other hand with predictions from formulas from the literature. The measurements fit well to the simulated and calculated values, except the ones at the lowest primary electron energies with an overvoltage below ˜ 2. The reason for this discrepancy is not clear yet and has to be clarified by further investigations. The results apply for any microanalyser - even with energy-dispersive X-ray spectrometry (EDS) detection - if the probe diameters, which might deviate from those of the JEOL JXA-8530F, at suitable analysing parameters are considered.

Supramolecular interactions in biologically relevant compounds. 2-Pyrazineformamide thiosemicarbazones and some products of their cyclization

NASA Astrophysics Data System (ADS)

Castiñeiras, Alfonso; García-Santos, Isabel; Nogueiras, Silvia; Rodríguez-González, Iria; Rodríguez-Riobó, Raúl

2014-09-01

Reaction of 2-cyanopyrazine with thiosemicarbazide or N-methylthiosemicarbazide afforded the (Z)-2-(amino(pyrazin-2-yl)methylene)hydrazinecarbothioamide (HPzAm4DH) and (Z)-2-(amino(pyrazin-2-yl)methylene)-N-methylhydrazine carbothioamide (HPzAm4M), respectively. (2Z,N‧E)-N‧-(4-Oxothiazolidin-2-ylidene)pyrazine-2-carbohydrazonamide (HPzAmot, 5) and (2Z,N‧E)-N‧-(3-methyl-4-oxothiazolidin-2-ylidene)pyrazine-2-carbohydrazonamide (MPzAmot, 7) have been synthesized from these thiosemicarbazones with chloroacetic or bromoacetic acids, using a conventional synthetic methodology and microwave-assisted organic reaction enhancement. The crystal structures of the thiosemicarbazones and their solvates [HPzAm4DHṡ1/2 MeOH (1), HPzAm4DHṡH2O (2), HPzAm4M (3), HPzAm4Mṡ2H2O (4)] and the 1,3-thiazolidin-4-ones (5 and 7) have been studied by X-ray diffractometry. All of the compounds were characterized by elemental analysis, mass spectrometry, FT-IR and 1H and 13C NMR spectroscopy. Several by-products have also been isolated in a crystalline form, namely 3-((Z,E)-N‧-(4-oxothiazolidin-2-ylidene)carbamohydrazonium-yl)pyrazin-1-ium dibromide monohydrate, (H3PzAmot)Br2ṡH2O (6), 2-((5-(pyrazin-2-yl)-1H-1,2,4-triazol-3-yl)thio)acetic acid, (H2Pz124ttAc) (8), 2-amino-5-(pyrazin-2-yl)-1,3,4-thiadiazol-3-ium chloride monohydrate, (HPz134tda)ClṡH2O (9), and 2-(methylamino)-5-(pyrazin-2-yl)-1,3,4-thiadiazol-3-ium chloride N-methyl-5-(pyrazin-2-yl)-1,3,4-thiadiazol-2-amine solvate, (HMPz134tda)Clṡ(MPz134tda) (10). The structures of these compounds were also analyzed by X-ray diffractometry. The microwave-assisted organic reaction method for synthesis is easy, convenient, and ecofriendly when compared to the traditional synthetic methods. Crystal analysis revealed that the compounds have extended 3D supramolecular networks through high levels of H-bonding and weak molecular interactions between the molecular moieties and solvent molecules. The novel synthons, which are sustained by Nsbnd H⋯N and Nsbnd H⋯O hydrogen bonding and other weak interactions, have been shown to assemble with 1,3-thizolidine-4-ones, 1,2,4-trizole, or 1,3,4-thiadiazole derivatives in a zigzag or herringbone architecture.

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 ...

POLYCYCLIC AROMATIC HYDROCARBON FORMATION IN OPPOSED FLOW DIFFUSION FLAMES OF ETHANE. (R825412)

EPA Science Inventory

Abstract

The effect of fuel-side carbon density on the levels of polycyclic aromatic hydrocarbon (PAH) formation in atmospheric pressure, opposed flow, ethane diffusion flames has been studied using heated micro-probe sampling and gas chromatography/mass spectrometry (...

FORMATION OF POLYCYCLIC AROMATIC HYDROCARBONS IN AN ATMOSPHERIC PRESSURE ETHYLENE DIFFUSION FLAME. (R825412)

EPA Science Inventory

Abstract

The microstructure of an atmospheric pressure, counterflow, sooting, flat, laminar ethylene diffusion flame has been studied experimentally by withdrawing samples from within the flame using a heated quartz microprobe coupled to an online gas chromatograph/mas...

p-type zinc-blende GaN on GaAs substrates

NASA Astrophysics Data System (ADS)

Lin, M. E.; Xue, G.; Zhou, G. L.; Greene, J. E.; Morkoç, H.

1993-08-01

We report p-type cubic GaN. The Mg-doped layers were grown on vicinal (100) GaAs substrates by plasma-enhanced molecular beam epitaxy. Thermally sublimed Mg was, with N2 carrier gas, fed into an electron-cyclotron resonance source. p-type zinc-blende-structure GaN films were achieved with hole mobilities as high as 39 cm2/V s at room temperature. The cubic nature of the films were confirmed by x-ray diffractometry. The depth profile of Mg was investigated by secondary ions mass spectroscopy.

Thermally Stable Nanocrystalline Steel

NASA Astrophysics Data System (ADS)

Hulme-Smith, Christopher Neil; Ooi, Shgh Woei; Bhadeshia, Harshad K. D. H.

2017-10-01

Two novel nanocrystalline steels were designed to withstand elevated temperatures without catastrophic microstructural changes. In the most successful alloy, a large quantity of nickel was added to stabilize austenite and allow a reduction in the carbon content. A 50 kg cast of the novel alloy was produced and used to verify the formation of nanocrystalline bainite. Synchrotron X-ray diffractometry using in situ heating showed that austenite was able to survive more than 1 hour at 773 K (500 °C) and subsequent cooling to ambient temperature. This is the first reported nanocrystalline steel with high-temperature capability.

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

Petrova, V. A.; Orekhov, A. S.; Chernyakov, D. D.

A method for preparing multilayer film composites based on chitosan has been developed by the example of polymer pairs: chitosan–hyaluronic acid, chitosan–alginic acid, and chitosan–carrageenan. The structure of the composite films is characterized by X-ray diffractometry and scanning electron microscopy. It is shown that the deposition of a solution of hyaluronic acid, alginic acid, or carrageenan on a chitosan gel film leads to the formation of a polyelectrolyte complex layer at the interface, which is accompanied by the ordering of chitosan chains in the surface region; the microstructure of this layer depends on the nature of contacting polymer pairs.

Unidirectional growth, rocking curve, linear and nonlinear optical properties of LPHCl single crystals

NASA Astrophysics Data System (ADS)

Kumar, P. Ramesh; Gunaseelan, R.; Raj, A. Antony; Selvakumar, S.; Sagayaraj, P.

2012-06-01

Nonlinear optical amino-acid single crystal of L-phenylalanine hydrochloride (LPHCl) was successfully grown by unidirectional Sankaranarayanan-Ramasamy (SR) method under ambient conditions for the first time. The grown single crystal was subjected to different characterization analyses in order to find out its suitability for device fabrication. The crystalline perfection was evaluated using high-resolution X-ray diffractometry. It is evident from the optical absorption study that crystal has excellent transmission in the entire visible region with its lower cut off wavelength around 290 nm.

Refractive indexes of (Al, Ga, In) as epilayers on InP for optoelectronic applications

NASA Astrophysics Data System (ADS)

Mondry, M. J.; Babic, D. I.; Bowers, J. E.; Coldren, L. A.

1992-06-01

MBE grown bulk and short period superlattices of (Al, Ga, In) As epilayers lattice matched to InP were characterized by double-crystal diffractometry and low-temperature photoluminescence. A reflection spectroscopy technique was used to determine the refractive index of (Al, Ga, In) As films as a function of wavelength. The measured data were fitted to a single-oscillator dispersion model and the model coefficients are given. The resulting expression can be used in the design of wave-guides, modulators, and other optical devices.

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

Allison, N.; Finch, A.A.; Tudhope, A.W.

The Sr/Ca of coral skeletons demonstrates potential as an indicator of sea surface temperatures (SSTs). However, the glacial-interglacial SST ranges predicted from Sr/Ca of fossil corals are usually higher than from other marine proxies. We observed infilling of secondary aragonite, characterized by high Sr/Ca ratios, along intraskeletal pores of a fossil coral from Papua New Guinea that grew during the penultimate deglaciation (130 {+-} 2 ka). Selective microanalysis of unaltered areas of the fossil coral indicates that SSTs at {approx}130 ka were {le} 1 C cooler than at present in contrast with bulk measurements (combining infilled and unaltered areas) whichmore » indicate a difference of 6-7 C. The analysis of unaltered areas of fossil skeletons by microprobe techniques may offer a route to more accurate reconstruction of past SSTs.« less

Formation of the lamellar structure in Group IA and IIID iron meteorites

NASA Technical Reports Server (NTRS)

Kowalik, J. A.; Williams, D. B.; Goldstein, J. I.

1988-01-01

Analytical EM, light microscopy, and electron microprobe analysis are used to study the lamellar plessite structure of Group IA and IIID iron meteorites. The alpha lamellae in IIID structures contained a compositional gradient from 6.1 + or - 0.7 wt pct Ni at the center of the alpha lamellae to 3.6 + or - 0.5 wt pct at the alpha/gamma interface. For the Group IA irons, compositions of 4 wt pct Ni in alpha and about 48 wt pct Ni in gamma are found. Convergent beam electron diffraction was used to characterize the orientation relations at the alpha/gamma interface in the lamellar regions of both Group IA and IIID. The phase transformations responsible for the observed lamellar structure in the IA and IIID chemical groups were also investigated.

Astigmatism correction of a non-imaging double spectrometer fitted with a 2D array detector

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

Yaney, P.P.; Ernst, S.L.; Blackshire, J.

1992-12-01

A SPEX 1401 double spectrometer was adapted for a liquid nitrogen cooled CCD detector to permit both spectral and spatial analysis of ceramic specimens in a laser Raman microprobe system. The exit image of the spectrometer suffers from astigmatism due to off-axis spherical mirrors. A cylindrical lens was added before the CCD to correct for the astigmatism. The spectrometer and several lenses were modeled using an optical ray tracing program to characterize the astigmatism and to optimize the locations of the lens and the detector. The astigmatism and the spot pattern sizes determined by the model were in good agreementmore » with he observed performance of the modified spectrometer-detector system. Typical spot patterns fell within the 23 {mu}m square pixel size.« less

Laser Welding Dissimilar Reflective Alloys

NASA Technical Reports Server (NTRS)

Mccay, M. H.; Gopinathan, S.; Kahlen, F.; Speigel, L.

1993-01-01

This project, jointly sponsored by Rocketdyne and CSTAR, involves the development of laser joining of materials which have heretofore been impractical to bond. Of particular interest are joints between stainless steel and copper and also aluminum 6061 to aluminum 2219. CSTAR has a unique opportunity in this area since both the process and development and diagnostics are of interest to industry. Initial results using the pulse tailored laser welding technique developed in CLA for joining crack sensitive materials have proven promising for the aluminum joints based upon metallurgical and electronic microprobe analysis. A declaration of success requires additional mechanical testing. A CW technique has been applied to the stainless-copper joining with some preliminary success. These joints are of significant interest for aeronautics and rocket propulsion applications and the project is expected to continue.

In situ extraction and analysis of volatile elements and molecules from carbonaceous chondrites

NASA Technical Reports Server (NTRS)

Hartmetz, C. P.; Gibson, E. K., Jr.; Blanford, G. E.

1991-01-01

A laser microprobe mass spectrometer was used to measure volatiles released, on a scale of 30-50 microns, from freshly broken, sawed, and weathered surfaces in fragments of the Allende, Murchison, Coolidge, Felix, and Orgueil carbonaceous chondrites. Samples were heated to about 120 C under a vacuum of 200 ntorr and illuminated with the focused beam of a Q-switched Nd:glass laser of variable energy output (0.1-1.0 J); the gases released were analyzed using a computer-controlled mass-selective detector. The results are presented in tables and graphs and discussed in detail, with particular attention to aqueous alteration; weathering; thermal metamorphism; the distribution of sulfur-bearing phases; and differences in the amounts of volatiles in matrix, inclusions, and chondrules.

Nature of the H chondrite parent body regolith - Evidence from the Dimmitt breccia

NASA Technical Reports Server (NTRS)

Rubin, A. E.; Scott, E. R. D.; Taylor, G. J.; Keil, K.; Allen, J. S. B.; Mayeda, T. K.; Clayton, R. N.; Bogard, D. D.

1983-01-01

Meteorite regolith breccias are clastic rocks which formed by lithification of fragmental regolith material that once resided at the surface of a meteorite parent body. A study is reported of the matrix and 21 clasts of various sizes (0.2-24 mm) in the Dimmitt H chondrite regolith breccia using petrographic and electron microprobe techniques. In addition, oxygen isotope studies of three clasts and instrumental neutron activation analysis (INAA) and Ar-39/Ar-40 age dating of one clast are reported. The Dimmitt meteorite was found about 1942 near Dimmitt, Texas. Attention is given to analytical procedures, the clastic matrix, equilibrated clasts, poikilitic melt-rock clast, clasts of different chondrite groups, graphite-magnetite aggregates, the origin of exotic clasts, and the complexity of parent body surfaces processes.

Interstellar grains within interstellar grains

NASA Technical Reports Server (NTRS)

Bernatowicz, Thomas J.; Amari, Sachiko; Zinner, Ernst K.; Lewis, Roy S.

1991-01-01

Five interstellar graphite spherules extracted from the Murchison carbonaceous meteorite are studied. The isotopic and elemental compositions of individual particles are investigated with the help of an ion microprobe, and this analysis is augmented with structural studies of ultrathin sections of the grain interiors by transmission electron microscopy. As a result, the following procedure for the formation of the interstellar graphite spherule bearing TiC crystals is inferred: (1) high-temperature nucleation and rapid growth of the graphitic carbon spherule in the atmosphere of a carbon-rich star, (2) nucleation and growth of TiC crystals during continued growth of the graphitic spherule and the accretion of TiC onto the spherule, (3) quenching of the graphite growth process by depletion of C or by isolation of the spherule before other grain types could condense.

Characterization of human kidney stones using micro-PIXE and RBS: a comparative study between two different populations.

PubMed

Pineda-Vargas, C A; Eisa, M E M; Rodgers, A L

2009-03-01

The micro-PIXE and RBS techniques are used to investigate the matrix as well as the trace elemental composition of calcium-rich human tissues on a microscopic scale. This paper deals with the spatial distribution of trace metals in hard human tissues such as kidney stone concretions, undertaken at the nuclear microprobe (NMP) facility. Relevant information about ion beam techniques used for material characterization will be discussed. Mapping correlation between different trace metals to extract information related to micro-regions composition will be illustrated with an application using proton energies of 1.5 and 3.0 MeV and applied to a comparative study for human kidney stone concretions nucleation region analysis from two different population groups (Sudan and South Africa).

Stress dependence of the Raman spectrum of polycrystalline barium titanate in presence of localized domain texture

NASA Astrophysics Data System (ADS)

Sakashita, Tatsuo; Deluca, Marco; Yamamoto, Shinsuke; Chazono, Hirokazu; Pezzotti, Giuseppe

2007-06-01

The stress dependence of the Raman spectrum of polycrystalline barium titanate (BaTiO3, BT) ceramics has been examined with microprobe polarized Raman spectroscopy. The angular dependence of the Raman spectrum of the tetragonal BT crystal has been theoretically established, enabling us to assess the stress dependence of selected spectral modes without the influence of crystallographic domain orientation. Upon considering the frequency shift of selected Raman modes as a function of orientation between the crystallographic axis and the polarization vector of incident and scattered light, a suitable instrumental configuration has been selected, which allowed a direct residual stress measurement according to a modified piezospectroscopic procedure. The analysis is based on the selection of mixed photostimulated spectral modes in two perpendicular angular orientations.

Electrochemical Atomic Layer Epitaxy of Thin Film CdSe

NASA Astrophysics Data System (ADS)

Pham, L.; Kaleida, K.; Happek, U.; Mathe, M. K.; Vaidyanathan, R.; Stickney, J. L.; Radevic, M.

2002-10-01

Electrochemical atomic layer epitaxy (EC-ALE) is a current developmental technique for the fabrication of compound semiconductor thin films. The deposition of elements making up the compound utilizes surface limited reactions where the potential is less than that required for bulk growth. This growth method offers mono-atomic layer control, allowing the deposition of superlattices with sharp interfaces. Here we report on the EC-ALE formation of CdSe thin films on Au and Cu substrates using an automated flow cell system. The band gap was measured using IR absorption and photoconductivity and found to be consistent with the literature value of 1.74 eV at 300K and 1.85 eV at 20K. The stoichiometry of the thin film was confirmed with electron microprobe analysis and x-ray diffraction.

Laser welding dissimilar reflective alloys

NASA Astrophysics Data System (ADS)

McCay, M. H.; Gopinathan, S.; Kahlen, F.; Speigel, L.

1993-01-01

This project, jointly sponsored by Rocketdyne and CSTAR, involves the development of laser joining of materials which have heretofore been impractical to bond. Of particular interest are joints between stainless steel and copper and also aluminum 6061 to aluminum 2219. CSTAR has a unique opportunity in this area since both the process and development and diagnostics are of interest to industry. Initial results using the pulse tailored laser welding technique developed in CLA for joining crack sensitive materials have proven promising for the aluminum joints based upon metallurgical and electronic microprobe analysis. A declaration of success requires additional mechanical testing. A CW technique has been applied to the stainless-copper joining with some preliminary success. These joints are of significant interest for aeronautics and rocket propulsion applications and the project is expected to continue.

Development of a new in-air micro-PIXE set-up with in-vacuum charge measurements in Atomki

NASA Astrophysics Data System (ADS)

Török, Zs.; Huszánk, R.; Csedreki, L.; Dani, J.; Szoboszlai, Z.; Kertész, Zs.

2015-11-01

A new external microbeam set-up has recently been installed as the extension of the existing microprobe system at the Laboratory of Ion Beam Applications of Atomki, Debrecen, Hungary. The external beam set-up, based on the system of Oxford Microbeams (OM), is equipped with two X-ray detectors for PIXE analysis, a digital microscope, two alignment lasers and a precision XYZ stage for easy and reproducible positioning of the sample. Exit windows with different thicknesses and of different materials can be used according to the actual demands, currently silicon-nitride (Si3N4) film with 200 nm thickness is employed in our laboratory. The first application was demonstrated in the field of archaeometry, on Bronze Age hoards from Hungary.

Analysis of Picosecond Pulsed Laser Melted Graphite

DOE R&D Accomplishments Database

Steinbeck, J.; Braunstein, G.; Speck, J.; Dresselhaus, M. S.; Huang, C. Y.; Malvezzi, A. M.; Bloembergen, N.

1986-12-01

A Raman microprobe and high resolution TEM have been used to analyze the resolidified region of liquid carbon generated by picosecond pulse laser radiation. From the relative intensities of the zone center Raman-allowed mode for graphite at 1582 cm{sup -1} and the disorder-induced mode at 1360 cm{sup -1}, the average graphite crystallite size in the resolidified region is determined as a function of position. By comparison with Rutherford backscattering spectra and Raman spectra from nanosecond pulsed laser melting experiments, the disorder depth for picosecond pulsed laser melted graphite is determined as a function of irradiating energy density. Comparisons of TEM micrographs for nanosecond and picosecond pulsed laser melting experiments show that the structure of the laser disordered regions in graphite are similar and exhibit similar behavior with increasing laser pulse fluence.

Modified extrusion-spheronization as a technique of microencapsulation for stabilization of choline bitartrate using hydrogenated soya bean oil

PubMed Central

Gangurde, Avinash Bhaskar; Sav, Ajay Kumar; Javeer, Sharadchandra Dagadu; Moravkar, Kailas K; Pawar, Jaywant N; Amin, Purnima D

2015-01-01

Introduction: Choline bitartrate (CBT) is a vital nutrient for fetal brain development and memory function. It is hygroscopic in nature which is associated with stability related problem during storage such as development of fishy odor and discoloration. Aim: Microencapsulation method was adopted to resolve the stability problem and for this hydrogenated soya bean oil (HSO) was used as encapsulating agent. Materials and Methods: Industrially feasible modified extrusion-spheronization technique was selected for microencapsulation. HSO was used as encapsulating agent, hydroxypropyl methyl cellulose E5/E15 as binder and microcrystalline cellulose as spheronization aid. Formulated pellets were evaluated for parameters such as flow property, morphological characteristics, hardness-friability index (HFI), drug content, encapsulation efficiency, and in vitro drug release. The optimized formulations were also characterized for particle size (by laser diffractometry), differential scanning calorimetry, powder X-ray diffractometry (PXRD), Fourier transform infrared spectroscopy, and scanning electron microscopy. Results and Discussions: The results from the study showed that coating of 90% and 60% CBT was successful with respect to all desired evaluation parameters. Optimized formulation was kept for 6 months stability study as per ICH guidelines, and there was no change in color, moisture content, drug content, and no fishy odor was observed. Conclusion: Microencapsulated pellets of CBT using HSO as encapsulating agent were developed using modified extrusion spheronization technique. Optimized formulations, CBT 90% (F5), and CBT 60% (F10), were found to be stable for 4M and 6M, respectively, at accelerated conditions. PMID:26682198

Rapid disintegrating tablets of simvastatin dispersions in polyoxyethylene–polypropylene block copolymer for maximized disintegration and dissolution

PubMed Central

Balata, Gehan F; Zidan, Ahmad S; Abourehab, Mohamad AS; Essa, Ebtessam A

2016-01-01

The objective of this research was to improve the dissolution of simvastatin and to incorporate it in rapid disintegrating tablets (RDTs) with an optimized disintegration and dissolution characteristics. Polyoxyethylene–polypropylene block copolymer (poloxamer 188) was employed as a hydrophilic carrier to prepare simvastatin solid dispersions (SDs). Fourier transform infrared spectroscopy, differential scanning calorimetry (DSC) and X-ray diffractometry were employed to understand the interaction between the drug and the carrier in the solid state. The results obtained from Fourier transform infrared spectroscopy showed absence of any chemical interaction between the drug and poloxamer. The results of differential scanning calorimetry and X-ray diffractometry confirmed the conversion of simvastatin to distorted crystalline state. The SD of 1:2 w/w drug to carrier ratio showed the highest dissolution; hence, it was incorporated in RDT formulations using a 32 full factorial design and response surface methodology. The initial assessments of RDTs demonstrated an acceptable flow, hardness, and friability to indicate good mechanical strength. The interaction and Pareto charts indicated that percentage of croscarmellose sodium incorporated was the most important factor affecting the disintegration time and dissolution parameter followed by the hardness value and their interaction effect. Compression force showed a superior influence to increase RDT’s porosity and to fasten disintegration rather than swelling action by croscarmellose sodium. On the other hand, croscarmellose sodium was most important for the initial simvastatin release. The results suggest the potential use of poloxamer 188-based SD in RDT for the oral delivery of poor water-soluble antihyperlipidemic drug, simvastatin. PMID:27757012

Spatial Distribution of Trehalose Dihydrate Crystallization in Tablets by X-ray Diffractometry.

PubMed

Thakral, Naveen K; Yamada, Hiroyuki; Stephenson, Gregory A; Suryanarayanan, Raj

2015-10-05

Crystallization of trehalose dihydrate (C12H22O11·2H2O) was induced by storing tablets of amorphous anhydrous trehalose (C12H22O11) at 65% RH (RT). Our goal was to evaluate the advantages and limitations of two approaches of profiling spatial distribution of drug crystallization in tablets. The extent of crystallization, as a function of depth, was determined in tablets stored for different time-periods. The first approach was glancing angle X-ray diffractometry, where the penetration depth of X-rays was modulated by the incident angle. Based on the mass attenuation coefficient of the matrix, the depth of X-ray penetration was calculated as a function of incident angle, which in turn enabled us to "calculate" the extent of crystallization to different depths. In the second approach, the tablets were split into halves and the split surfaces were analyzed directly. Starting from the tablet surface and moving toward the midplane, XRD patterns were collected in 36 "regions", in increments of 0.05 mm. The results obtained by the two approaches were, in general, in good agreement. Additionally, the results obtained were validated by determining the "average" crystallization in the entire tablet by using synchrotron radiation in the transmission mode. The glancing angle method could detect crystallization up to ∼650 μm and had a "surface bias". Being a nondestructive technique, this method will permit repeated analyses of the same tablet at different time points, for example, during a stability study. However, split tablet analyses, while a "destructive" technique, provided comprehensive and unbiased depth profiling information.

Clusters of Defects in Semiconductors

DTIC Science & Technology

1984-08-01

onecionbewen-te heica seces .-. o* Fe and.th deec prd *n th *Rlmnecne ae t..* E. STATISTICS The funds from this contract were used to support the research of...characterized at Hughes Research Laboratories. L x No Np N1 . Electron X-ray Sample (cm- 1) (cm- ) (cm-3 ) microprobe Density diffraction .. -. C077 3.6x 10

Electron multiplier-ion detector system

DOEpatents

Dietz, L.A.

1975-08-01

This patent relates to an improved ion detector for use in mass spectrometers for pulse counting signal ions which may have a positive or a negative charge. The invention combines a novel electron multiplier with a scintillator type of ion detector. It is a high vacuum, high voltage device intended for use in ion microprobe mass spectrometers. (auth)

Spinel from Apollo 12 Olivine Mare Basalts: Chemical Systematics of Selected Major, Minor, and Trace Elements

NASA Technical Reports Server (NTRS)

Papike, J. J.; Karner, J. M.; Shearer, C. K.; Spilde, M. N.

2002-01-01

Spinels from Apollo 12 Olivine basalts have been studied by Electron and Ion microprobe techniques. The zoning trends of major, minor and trace elements provide new insights into the conditions under which planetary basalts form. Additional information is contained in the original extended abstract.

KSC-98pc1626

NASA Image and Video Library

1998-11-10

KENNEDY SPACE CENTER, FLA. -- In the Spacecraft Assembly and Encapsulation Facility -2 (SAEF-2), workers from the Jet Propulsion Laboratory open the drums containing the Mars microprobes that will hitchhike on the Mars Polar Lander. From left, they are Satish Krishnan, Charles Cruzan, Chris Voorhees and Arden Acord. Scheduled to be launched Jan. 3, 1999, aboard a Delta II rocket, the solar-powered spacecraft is designed to touch down on the Martian surface near the northern-most boundary of the south pole in order to study the water cycle there. The lander also will help scientists learn more about climate change and current resources on Mars, studying such things as frost, dust, water vapor and condensates in the Martian atmosphere. The Mars microprobes, called Deep Space 2, are part of NASA's New Millennium Program. They will complement the climate-related scientific focus of the lander by demonstrating an advanced, rugged microlaser system for detecting subsurface water. Such data on polar subsurface water, in the form of ice, should help put limits on scientific projections for the global abundance of water on Mars

Deep Space 2: The Mars Microprobe Mission

NASA Astrophysics Data System (ADS)

Smrekar, Suzanne; Catling, David; Lorenz, Ralph; Magalhães, Julio; Moersch, Jeffrey; Morgan, Paul; Murray, Bruce; Presley-Holloway, Marsha; Yen, Albert; Zent, Aaron; Blaney, Diana

The Mars Microprobe Mission will be the second of the New Millennium Program's technology development missions to planetary bodies. The mission consists of two penetrators that weigh 2.4 kg each and are being carried as a piggyback payload on the Mars Polar Lander cruise ring. The spacecraft arrive at Mars on December 3, 1999. The two identical penetrators will impact the surface at ~190 m/s and penetrate up to 0.6 m. They will land within 1 to 10 km of each other and ~50 km from the Polar Lander on the south polar layered terrain. The primary objective of the mission is to demonstrate technologies that will enable future science missions and, in particular, network science missions. A secondary goal is to acquire science data. A subsurface evolved water experiment and a thermal conductivity experiment will estimate the water content and thermal properties of the regolith. The atmospheric density, pressure, and temperature will be derived using descent deceleration data. Impact accelerometer data will be used to determine the depth of penetration, the hardness of the regolith, and the presence or absence of 10 cm scale layers.

Enhanced Raman Microprobe Imaging of Single-Wall Carbon Nanotubes

NASA Technical Reports Server (NTRS)

Hadjiev, V. G.; Arepalli, S.; Nikolaev, P.; Jandl, S.; Yowell, L.

2003-01-01

We explore Raman microprobe capabilities to visualize single wall carbon nanotubes (SWCNTs). Although this technique is limited to a micron scale, we demonstrate that images of individual SWCNTs, bundles or their agglomerates can be generated by mapping Raman active elementary excitations. We measured the Raman response from carbon vibrations in SWCNTs excited by confocal scanning of a focused laser beam. Carbon vibrations reveal key characteristics of SWCNTs as nanotube diameter distribution (radial breathing modes, RBM, 100-300 cm(exp -1)), presence of defects and functional groups (D-mode, 1300-1350 cm(exp -1)), strain and oxidation states of SWCNTs, as well as metallic or semiconducting character of the tubes encoded in the lineshape of the G-modes at 1520-1600 cm(exp - 1). In addition, SWCNTs are highly anisotropic scatterers. The Raman response from a SWCNT is maximal for incident light polarization parallel to the tube axis and vanishing for perpendicular directions. We show that the SWCNT bundle shape or direction can be determined, with some limitations, from a set of Raman images taken at two orthogonal directions of the incident light polarization.

TEAM - Titan Exploration Atmospheric Microprobes

NASA Astrophysics Data System (ADS)

Nixon, Conor; Esper, Jaime; Aslam, Shahid; Quilligan, Gerald

2016-10-01

The astrobiological potential of Titan's surface hydrocarbon liquids and probable interior water ocean has led to its inclusion as a destination in NASA's "Ocean Worlds" initiative, and near-term investigation of these regions is a high-level scientific goal. TEAM is a novel initiative to investigate the lake and sea environs using multiple dropsondes -scientific probes derived from an existing cubesat bus architecture (CAPE - the Cubesat Application for Planetary Exploration) developed at NASA GSFC. Each 3U probe will parachute to the surface, making atmospheric structure and composition measurements during the descent, and photographing the surface - land, shoreline and seas - in detail. TEAM probes offer a low-cost, high-return means to explore multiple areas on Titan, yielding crucial data about the condensing chemicals, haze and cloud layers, winds, and surface features of the lakes and seas. These microprobes may be included on a near-term New Frontiers class mission to the Saturn system as additional payload, bringing increased scientific return and conducting reconnaissance for future landing zones. In this presentation we describe the probe architecture, baseline payload, flight profile and the unique engineering and science data that can be returned.

Oxidation characteristics of Ti-25Al-10Nb-3V-1Mo intermetallic alloy

NASA Technical Reports Server (NTRS)

Wallace, Terryl A.; Clark, Ronald K.; Sankaran, Sankara N.; Wiedemann, Karl E.

1990-01-01

Static oxidation kinetics of the super-alpha 2 titanium-aluminide alloy Ti-25Al-10Nb-3V-1Mo (at. percent) were investigated in air over the temperature range of 650 to 1000 C using thermogravimetric analysis. The oxidation kinetics were complex at all exposure temperatures and displayed up to three distinct oxidation rates. Breakaway oxidation occurred after long exposure times at high temperatures. Oxidation products were determined using x ray diffraction techniques, electron microprobe analysis, and energy dispersive x ray analysis. Oxide scale morphology was examined by scanning electron microscopy of the surfaces and cross sections of oxidized specimens. The oxides during the parabolic stages were compact and multilayered, consisting primarily of TiO2 doped with Nb, a top layer of Al2O3, and a thin bottom layer of TiN. The transition between the second and third parabolic stage was found to be linked to the formation of a TiAl layer at the oxide-metal interface. Porosity was formed during the third stage, causing degradation of the oxide and the beginning of breakaway oxidation.

Microbiologically influenced corrosion: looking to the future.

PubMed

Videla, Héctor A; Herrera, Liz K

2005-09-01

This review discusses the state-of-the-art of research into biocorrosion and the biofouling of metals and alloys of industrial usage. The key concepts needed to understand the main effects of microorganisms on metal decay, and current trends in monitoring and control strategies to mitigate the deleterious effects of biocorrosion and biofouling are also described. Several relevant cases of biocorrosion studied by our research group are provided as examples: (i) biocorrosion of aluminum and its alloys by fungal contaminants of jet fuels; (ii) sulfate-reducing bacteria (SRB)-induced corrosion of steel; (iii) biocorrosion and biofouling interactions in the marine environment; (iv) monitoring strategies for assessing biocorrosion in industrial water systems; (v) microbial inhibition of corrosion; (vi) use and limitations of electrochemical techniques for evaluating biocorrosion effects. Future prospects in the field are described with respect to the potential of innovative techniques in microscopy (environmental scanning electron microscopy, confocal scanning laser microscopy, atomic force microscopy), new spectroscopic techniques for the study of corrosion products and biofilms (energy dispersion X-ray analysis, X-ray photoelectron spectroscopy, electron microprobe analysis) and electrochemistry (electrochemical impedance spectroscopy, electrochemical noise analysis).

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

Not Available

The methods cover: C in solutions, F (electrode), elements by atomic emission spectrometry, inorganic anions by ion chromatography, Hg in water/solids/sludges, As, Se, Bi, Pb, data calculations for SST (single shell tank?) samples, Sb, Tl, Ag, Pu, O/M ratio, ignition weight loss, pH value, ammonia (N), Cr(VI), alkalinity, U, C sepn. from soil/sediment/sludge, Pu purif., total N, water, C and S, surface Cl/F, leachable Cl/F, outgassing of Ge detector dewars, gas mixing, gas isotopic analysis, XRF of metals/alloys/compounds, H in Zircaloy, H/O in metals, inpurity extraction, reduced/total Fe in glass, free acid in U/Pu solns, density of solns, Kr/Xe isotopesmore » in FFTF cover gas, H by combustion, MS of Li and Cs isotopes, MS of lanthanide isotopes, GC operation, total Na on filters, XRF spectroscopy QC, multichannel analyzer operation, total cyanide in water/solid/sludge, free cyanide in water/leachate, hydrazine conc., ICP-MS, {sup 99}Tc, U conc./isotopes, microprobe analysis of solids, gas analysis, total cyanide, H/N{sub 2}O in air, and pH in soil.« less

Interdiffusion behavior of tungsten or rhenium and group 5 and 6 elements and alloys of the periodic table, part 1. [at dissimilar metal joints

NASA Technical Reports Server (NTRS)

Arcella, F. G.

1974-01-01

Arc cast W, CVD W, CVD Re, and powder metallurgy Re materials were hot isostatically pressure welded to ten different refractory metals and alloys (Cb, Cb-1Zr, Ta, Ta-10W, T-111, ASTAR-811C, W-25Re, Mo-50Re, W-30Re-20Mo, ect.) and thermally aged at 10 to the minus 8th power torr at 1200, 1500, 1630, 1800, and 2000 C for 100 to 2000 hours. Electron beam microprobe analysis was used to characterize the interdiffusion zone width of each couple system as a function of age time and temperature. Extrapolations of interdiffusion zone thickness to 10,000 hours were made. Classic interdiffusion analysis was performed for several of the systems by Boltzmann-Matano analysis. A method of inhibiting Kirkendall voids from forming during thermal ageing of dissimilar metal junctions was devised and experimentally demonstrated. An electron beam weld study of Cb-1Zr to Re and W-25Re demonstrated the limited acceptability of these welds.

Growth of diamond by RF plasma-assisted chemical vapor deposition

NASA Technical Reports Server (NTRS)

Meyer, Duane E.; Ianno, Natale J.; Woollam, John A.; Swartzlander, A. B.; Nelson, A. J.

1988-01-01

A system has been designed and constructed to produce diamond particles by inductively coupled radio-frequency, plasma-assisted chemical vapor deposition. This is a low-pressure, low-temperature process used in an attempt to deposit diamond on substrates of glass, quartz, silicon, nickel, and boron nitride. Several deposition parameters have been varied including substrate temperature, gas concentration, gas pressure, total gas flow rate, RF input power, and deposition time. Analytical methods employed to determine composition and structure of the deposits include scanning electron microscopy, absorption spectroscopy, scanning Auger microprobe spectroscopy, and Raman spectroscopy. Analysis indicates that particles having a thin graphite surface, as well as diamond particles with no surface coatings, have been deposited. Deposits on quartz have exhibited optical bandgaps as high as 4.5 eV. Scanning electron microscopy analysis shows that particles are deposited on a pedestal which Auger spectroscopy indicates to be graphite. This is a phenomenon that has not been previously reported in the literature.

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

Nieroda, Pawel; Zybala, Rafal; Wojciechowski, Krzysztof T.

The aim of the study was to develop a fast and simple method for preparation of polycrystalline Mg{sub 2}Si. For this purpose a Spark Plasma Sintering (SPS) method was used and synthesis conditions were adjusted in such a manner that no excess Mg was required. Materials were synthesized by the direct reaction of Mg and Si raw powders. To determine the phase and chemical composition, the fabricated samples were studied by X-ray diffraction and SEM microscopy coupled with EDX chemical analysis. Thermoelectric properties of samples (thermal conductivity, electrical conductivity and Seebeck coefficient) were measured all over temperature range of 300-650more » K. The analysis by the scanning thermoelectric microprobe (STM) shows that samples have uniform distribution of Seebeck coefficient with mean value of about -405 {mu}VK{sup -1} and standard deviation of 94 {mu}VK{sup -1}. Prepared materials have intrinsic band gap of 0.45 eV and thermal conductivity {lambda}= 7.5 Wm{sup -1}K{sup -1} at room temperature.« less

Radiative properties of advanced spacecraft heat shield materials

NASA Technical Reports Server (NTRS)

Cunnington, G. R.; Funai, A. I.; Mcnab, T. K.

1983-01-01

Experimental results are presented to show the effects of simulated reentry exposure by convective heating and by radiant heating on spectral and total emittance of statically oxidized Inconel 617 and Haynes HS188 superalloys to 1260 K and a silicide coatea (R512E) columbium 752 alloy to 1590 K. Convective heating exposures were conducted in a supersonic arc plasma wind tunnel using a wedge-shaped specimen configuration. Radiant tests were conducted at a pressure of .003 atmospheres of dry air at a flow velocity of several meters per second. Convective heating specimens were subjected to 8, 20, and 38 15-min heating cycles, and radiant heating specimens were tested for 10, 20, 50, and 100 30-min heating cycles. Changes in radiative properties are explained in terms of changes in composition resulting from simulated reentry tests. The methods used to evaluate morphological, compositional and crystallographic changes include: Auger electron spectroscopy; scanning electron microscopy; X-ray diffraction analysis; and electron microprobe analysis.

Enhanced Carbon Diffusion in Austenitic Stainless Steel Carburized at Low Temperature

NASA Astrophysics Data System (ADS)

Ernst, F.; Avishai, A.; Kahn, H.; Gu, X.; Michal, G. M.; Heuer, A. H.

2009-08-01

Austenitic stainless steel AISI 316L was carburized by a novel, low-temperature gas-phase process. Using a calibrated scanning Auger microprobe (SAM) analysis of cross-sectional specimens under dynamic sputtering, we determined the fraction-depth profile of carbon. The profile is concave—very different from the shape expected for concentration-independent diffusion—and indicates a carbide-free solid solution with carbon levels up to 15 at. pct and a case depth of ≈30 μm. A Boltzmann-Matano analysis with a careful evaluation of the stochastic and potential systematic errors indicates that increasing levels of carbon significantly enhance carbon diffusion. For the highest carbon level observed (15 at. pct), the carbon diffusion coefficient is more than two orders of magnitude larger than in dilute solution. The most likely explanation for this strong increase is that carbon-induced local expansion of metal-metal atom distances, observed as an expansion of the lattice parameter, reduces the activation energy for carbon diffusion.

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

Kelli Kazuberns; Sushil Gupta; Mihaela Grigore

Blast furnace efficiency may be improved by optimizing coke reactivity. Some but not all forms of mineral matter in the coke modify its reactivity, but changes in mineral matter that occur within coke while in the blast furnace have not been fully quantified. To determine changes in mineral matter forms in the blast furnace, coke samples from a dissection study in the LKAB experimental blast furnace (EBF) were characterized using SEM/EDS analysis, EPMA (microprobe), and low-temperature ashing/quantitative XRD analysis. Variations in alkali concentration, particularly potassium, dominated the compositional changes. At high concentrations of potassium, the mineral matter was largely potassium-bearingmore » but even more potassium was diffused throughout the coke and not associated with mineral matter. There was little difference in potassium concentration between the core and surface of the coke pieces, suggesting that potassium diffused rapidly through the whole coke. Iron, calcium, silicon, and aluminum concentrations were relatively constant in comparison, although the mineralogy of all elements changed significantly with changing temperature. 23 refs., 20 figs., 9 tabs.« less

Aluminium alloys in municipal solid waste incineration bottom ash.

PubMed

Hu, Yanjun; Rem, Peter

2009-05-01

With the increasing growth of incineration of household waste, more and more aluminium is retained in municipal solid waste incinerator bottom ash. Therefore recycling of aluminium from bottom ash becomes increasingly important. Previous research suggests that aluminium from different sources is found in different size fractions resulting in different recycling rates. The purpose of this study was to develop analytical and sampling techniques to measure the particle size distribution of individual alloys in bottom ash. In particular, cast aluminium alloys were investigated. Based on the particle size distribution it was computed how well these alloys were recovered in a typical state-of-the-art treatment plant. Assessment of the cast alloy distribution was carried out by wet physical separation processes, as well as chemical methods, X-ray fluorescence analysis and electron microprobe analysis. The results from laboratory analyses showed that cast alloys tend to concentrate in the coarser fractions and therefore are better recovered in bottom ash treatment plants.

Heat pipe fatigue test specimen: Metallurgical evaluation

NASA Technical Reports Server (NTRS)

Walak, Steven E.; Cronin, Michael J.; Grobstein, Toni

1992-01-01

An innovative creep/fatigue test was run to simulate the temperature, mechanical load, and sodium corrosion conditions expected in a heat pipe designed to supply thermal energy to a Stirling cycle power converter. A sodium-charged Inconel 718 heat pipe with a Nickel 200 screen wick was operated for 1090 hr at temperatures between 950 K (1250 F) and 1050 K (1430 F) while being subjected to creep and fatigue loads in a servo-hydraulic testing machine. After testing, the heat pipe was sectioned and examined using optical microscopy, scanning electron microscopy, and electron microprobe analysis with wavelength dispersive x-ray spectroscopy. The analysis concentrated on evaluating topographic, microstructural, and chemical changes in the sodium exposed surfaces of the heat pipe wall and wick. Surface changes in the evaporator, condenser, and adiabatic sections of the heat pipe were examined in an effort to correlate the changes with the expected sodium environment in the heat pipe. This report describes the setup, operating conditions, and analytical results of the sodium heat pipe fatigue test.

Dual Source Time-of-flight Mass Spectrometer and Sample Handling System

NASA Astrophysics Data System (ADS)

Brinckerhoff, W.; Mahaffy, P.; Cornish, T.; Cheng, A.; Gorevan, S.; Niemann, H.; Harpold, D.; Rafeek, S.; Yucht, D.

We present details of an instrument under development for potential NASA missions to planets and small bodies. The instrument comprises a dual ionization source (laser and electron impact) time-of-flight mass spectrometer (TOF-MS) and a carousel sam- ple handling system for in situ analysis of solid materials acquired by, e.g., a coring drill. This DSTOF instrument could be deployed on a fixed lander or a rover, and has an open design that would accommodate measurements by additional instruments. The sample handling system (SHS) is based on a multi-well carousel, originally de- signed for Champollion/DS4. Solid samples, in the form of drill cores or as loose chips or fines, are inserted through an access port, sealed in vacuum, and transported around the carousel to a pyrolysis cell and/or directly to the TOF-MS inlet. Samples at the TOF-MS inlet are xy-addressable for laser or optical microprobe. Cups may be ejected from their holders for analyzing multiple samples or caching them for return. Samples are analyzed with laser desorption and evolved-gas/electron-impact sources. The dual ion source permits studies of elemental, isotopic, and molecular composition of unprepared samples with a single mass spectrometer. Pulsed laser desorption per- mits the measurement of abundance and isotope ratios of refractory elements, as well as the detection of high-mass organic molecules in solid samples. Evolved gas analysis permits similar measurements of the more volatile species in solids and aerosols. The TOF-MS is based on previous miniature prototypes at JHU/APL that feature high sensitivity and a wide mass range. The laser mode, in which the sample cup is directly below the TOF-MS inlet, permits both ablation and desorption measurements, to cover elemental and molecular species, respectively. In the evolved gas mode, sample cups are raised into a small pyrolysis cell and heated, producing a neutral gas that is elec- tron ionized and pulsed into the TOF-MS. (Any imaging and laser microprobe studies would necessarily precede the pyrolysis step to assure that the grain-scale composition is captured.)

Robust Extraction and Multi-Technique Analysis of Micrometeoroids Captured in Low Earth Orbit

NASA Technical Reports Server (NTRS)

Westphal, A. J.; Graham, G. A.; Bench, G.; Brennan, S.; Luening, K.; Pianetta, P.; Keller, L. P.; Flynn, G. J.; Snead, C.; Dominquez, G.

2003-01-01

The use of low-density silica aerogel as the primary capture cell technology for the NASA Discovery mission Stardust to Comet Wild-2 [1] is a strong motivation for researchers within the Meteoritics community to develop techniques to handle this material. The unique properties of silica aerogel allow dust particles to be captured at hypervelocity speeds and to remain partially intact. The same unique properties present difficulties in the preparation of particles for analysis. Using tools borrowed from microbiologists, we have developed techniques for robustly extracting captured hypervelocity dust particles and their residues from aerogel collectors[2-3]. It is important not only to refine these extraction techniques but also to develop protocols for analyzing the captured particles. Since Stardust does not return material to Earth until 2006, researchers must either analyze particles that are impacted in the laboratory using light-gasgun facilities [e.g. 41 or examine aerogel collectors that have been exposed in low-Earth orbit (LEO) [5]. While there are certainly benefits in laboratory shots, i.e. accelerating known compositions of projectiles into aerogel, the LEO capture particles offer the opportunity to investigate real particles captured under real conditions. The aerogel collectors used in this research are part of the NASA Orbital Debris Collection Experiment that was exposed on the MIR Space Station for 18 months [5]. We have developed the capability at the UCB Space Sciences Laboratory to extract tiny volumes of aerogel that completely contain each impact event, and to mount them on micromachined fixtures so that they can be analyzed with no interfering support (Fig.1). These aerogel keystones simultaneously bring the terminal particle and the particle track to within 10 m (15 g cm- ) of the nearest aerogel surface. The extracted aerogel wedges containing both the impact tracks and the captured particles have been characterized using the synchrotron total external reflection X-ray fluorescence (TXRF) microprobe at SSRL, the Nuclear Microprobe at LLNL, synchrotron infrared microscopy at the ALS facility at LBL and the NSLS at BNL, and the Total Reflection X-ray Fluorescence (TXRF) facility at SLAC.

Energy dispersive X-ray fluorescence spectroscopy/Monte Carlo simulation approach for the non-destructive analysis of corrosion patina-bearing alloys in archaeological bronzes: The case of the bowl from the Fareleira 3 site (Vidigueira, South Portugal)

NASA Astrophysics Data System (ADS)

Bottaini, C.; Mirão, J.; Figuereido, M.; Candeias, A.; Brunetti, A.; Schiavon, N.

2015-01-01

Energy dispersive X-ray fluorescence (EDXRF) is a well-known technique for non-destructive and in situ analysis of archaeological artifacts both in terms of the qualitative and quantitative elemental composition because of its rapidity and non-destructiveness. In this study EDXRF and realistic Monte Carlo simulation using the X-ray Monte Carlo (XRMC) code package have been combined to characterize a Cu-based bowl from the Iron Age burial from Fareleira 3 (Southern Portugal). The artifact displays a multilayered structure made up of three distinct layers: a) alloy substrate; b) green oxidized corrosion patina; and c) brownish carbonate soil-derived crust. To assess the reliability of Monte Carlo simulation in reproducing the composition of the bulk metal of the objects without recurring to potentially damaging patina's and crust's removal, portable EDXRF analysis was performed on cleaned and patina/crust coated areas of the artifact. Patina has been characterized by micro X-ray Diffractometry (μXRD) and Back-Scattered Scanning Electron Microscopy + Energy Dispersive Spectroscopy (BSEM + EDS). Results indicate that the EDXRF/Monte Carlo protocol is well suited when a two-layered model is considered, whereas in areas where the patina + crust surface coating is too thick, X-rays from the alloy substrate are not able to exit the sample.

Study of polycation effects on erythrocyte agglutination mediated by anti-glycophorins using microscopic image digital analysis

NASA Astrophysics Data System (ADS)

Riquelme, B.; Dumas, D.; Relancio, F.; Fontana, A.; Alessi, A.; Foresto, P.; Grandfils, C.; Stoltz, J.; Valverde, J.

2006-04-01

The aim of this work was to study synthetic polycation effects on erythrocyte agglutination mediated by anti-glycophorin using image digital analysis. Polycations are oligomers or polymers of natural or synthetic origin, which bear a great number of positive charges at pH 7.4. Several of these polycations are nowadays used in clinic for human and veterinary purposes. New applications of polycations to the development of new drug delivery systems are investigated, in order to promote the drug absorption through the gastro-intestinal and blood brain barriers. However, up to now, there are no clear relationships between macromolecular features of polycations (molecular weight, mean charge density, charge repartition, etc.) and their interactions with blood elements (which bear superficial negative charges). The interaction on the red blood cell membrane with synthetic polycations having well-controlled macromolecular features and functionalized with pendent polyethylene glycol segments was investigated. The alterations over stationary and dynamic viscoelastic properties of erythrocyte membranes were analyzed through laser diffractometry. Image digital analysis was used to study erythrocyte agglutination mediated by anti-glycophorin. Results show different reactivities of the polycations on the erythrocyte membrane. These findings could provide more information about the mechanisms of polycation interaction on erythrocyte membranes. We consider that this work could provide useful tools to understand and improve the haemocompatibility of polycations and enlarge their potential in clinic.

Differentiations of Chitin Content and Surface Morphologies of Chitins Extracted from Male and Female Grasshopper Species

PubMed Central

Kaya, Murat; Lelešius, Evaldas; Nagrockaitė, Radvilė; Sargin, Idris; Arslan, Gulsin; Mol, Abbas; Baran, Talat; Can, Esra; Bitim, Betul

2015-01-01

In this study, we used Fourier transform infrared spectroscopy (FT-IR), elemental analysis (EA), thermogravimetric analysis (TGA), X-ray diffractometry (XRD), and scanning electron microscopy (SEM) to investigate chitin structure isolated from both sexes of four grasshopper species. FT-IR, EA, XRD, and TGA showed that the chitin was in the alpha form. With respect to gender, two main differences were observed. First, we observed that the quantity of chitin was greater in males than in females and the dry weight of chitin between species ranged from 4.71% to 11.84%. Second, using SEM, we observed that the male chitin surface structure contained 25 – 90nm wide nanofibers and 90 – 250 nm nanopores, while no pores or nanofibers were observed in the chitin surface structure of the majority of females (nanofibers were observed only in M. desertus females). In contrast, the elemental analysis, thermal properties, and crystalline index values for chitin were similar in males and females. Also, we carried out enzymatic digestion of the isolated chitins using commercial chitinase from Streptomyces griseus. We observed that there were no big differences in digestion rate of the chitins from both sexes and commercial chitin. The digestion rates were for grasshoppers’ chitins; 88.45–95.48% and for commercial chitin; 94.95%. PMID:25635814

Influence of beta-cyclodextrin complexation on glipizide release from hydroxypropyl methylcellulose matrix tablets.

PubMed

Shivakumar, H N; Desai, B G; Pandya, Saumyak; Karki, S S

2007-01-01

Glipizide was complexed with beta-cyclodextrin in an attempt to enhance the drug solubility. The phase solubility diagram was classified as A(L) type, which was characterized by an apparent 1:1 stability constant that had a value of 413.82 M(-1). Fourier transform infrared spectrophotometry, differential scanning calorimetry, powder x-ray diffractometry and proton nuclear magnetic resonance spectral analysis indicated considerable interaction between the drug and beta-cyclodextrin. A 2(3) factorial design was employed to prepare hydroxypropyl methylcellulose (HPMC) matrix tablets containing the drug or its complex. The effect of the total polymer loads (X1), levels of HPMC K100LV (X9), and complexation (X3) on release at first hour (Y1), 24 h (Y2), time taken for 50% release (Y3), and diffusion exponent (Y4) was systematically analyzed using the F test. Mathematical models containing only the significant terms (P < 0.05) were generated for each parameter by multiple linear regression analysis and analysis of variance. Complexation was found to exert a significant effect on Y1, Y2, and Y3, whereas total polymer loads significantly influenced all the responses. The models generated were validated by developing two new formulations with a combination of factors within the experimental domain. The experimental values of the response parameters were in close agreement with the predicted values, thereby proving-the validity of the generated mathematical models.

Evaluation of the diffusion of Mn, Fe, Ba and Pb in Middle Ages human teeth by synchrotron microprobe X-ray fluorescence

NASA Astrophysics Data System (ADS)

Carvalho, M. L.; Marques, A. F.; Marques, J. P.; Casaca, C.

2007-07-01

Human teeth from the Middle Ages have been analysed using a synchrotron microprobe evaluating Mn, Fe, Ba and Pb diffusion from the soil into the tooth structure. It is apparent that post-mortem teeth of ancient populations are influenced by the endogenous environment. The diffusion pattern of some elements can give information both for archaeological purposes and diagenesis processes affecting the apatite ante-mortem elemental content. An X-ray fluorescence set-up with microprobe capabilities, 100 μm of spatial resolution and energy of 18 keV, installed at LURE synchrotron (France) was used. Line scans were performed along the several regions of the teeth, in steps of 100 to 1000 μm. Ba is much enriched in ancient teeth when compared to recent ones, where this element is almost non-existent. Furthermore, the concentration profiles show increased levels of this element close to the external enamel region, reaching values up to 200 μg g - 1 decreasing in dentine and achieving a steady level in the inner dentine and root. Pb concentration profiles show strongly increased levels of this element close to the external enamel region (20 μg g - 1 ), decreasing strongly to the inner part of the dentine (0.5 μg g - 1 ) contrarily to the normal situation in modern citizens where the highest concentrations for Pb are in the inner root dentine. This behaviour suggests post-mortem uptake from the soil; the presence of elevated levels of Pb can be explained by the fact that this burial place was a car park for more than 20 years. The distribution of Mn and Fe follow very similar patterns and both are very much enriched especially in the outer surfaces in contact with the soil, showing strong contamination from the soil.

Increasing the Efficiency of Electron Microprobe Measurements of Minor and Trace Elements in Rutile

NASA Astrophysics Data System (ADS)

Neill, O. K.; Mattinson, C. G.; Donovan, J.; Hernández Uribe, D.; Sains, A.

2016-12-01

Minor and trace element contents of rutile, an accessory mineral found in numerous lithologic settings, has many applications for interpreting earth systems. While these applications vary widely, they share a need for precise and accurate elemental measurements. The electron microprobe can be used to measure rutile compositions, although long X-ray counting times are necessary to achieve acceptable precision. Continuum ("background") intensity can be estimated using the iterative Mean Atomic Number (MAN) method of Donovan and Tingle (1996), obviating the need for direct off-peak background measurements, and reducing counting times by half. For this study, several natural and synthetic rutiles were measured by electron microprobe. Data was collected once but reduced twice, using off-peak and an MAN background corrections, allowing direct comparison of the two methods without influence of other variables (counting time, analyte homogeneity, beam current, calibration standards, etc.). These measurements show that, if a "blank" correction (Donovan et al., 2011, 2016) is used, minor and trace elements of interest can be measured in rutile using the MAN background method in half the time of traditional off-peak measurements, without sacrificing accuracy or precision (Figure 1). This method has already been applied to Zr-in-rutile thermometry of ultra-high pressure metamorphic rocks from the North Qaidam terrane in northwest China. Finally, secondary fluorescence of adjacent phases by continuum X-rays can lead to artificially elevated concentrations. For example, when measuring Zr, care should be taken to avoid analytical spots within 100 microns of zircon or baddeleyite crystals. References: 1) J.J. Donovan and T.N Tingle (1996) J. Microscopy, 2(1), 1-7 2) J.J. Donovan, H.A. Lowers, and B.G. Rusk (2011) Am. Mineral., 96, 274­282 3) J.J. Donovan, J.W. Singer and J.T. Armstrong (2016) Am. Mineral., 101, 1839-1853 4) G.L. Lovizotto et al. (2009) Chem. Geol., 261, 346-369

Relationship between crystal structure and solid-state properties of pharmaceuticals

NASA Astrophysics Data System (ADS)

Sheth, Agam R.

This thesis strives to understand the structure-property relationships of some pharmaceutical crystals at the molecular level with emphasis on the effect of secondary processing on the solid phase. Using single crystal X-ray diffractometry (SCXRD), the structure of warfarin sodium 2-propanol adduct (W) was established to be a true solvate, contrary to previous reports. Using dynamic water vapor sorption, optical and environmental scanning electron microscopy, SCXRD, powder X-ray diffractometry (PXRD), volume computations and molecular modeling, the effect of relative humidity and temperature on the crystal structure of W was investigated. Ab initio calculations on piroxicam showed that the difference in energy between the two polymorphs, I and II, arises predominantly from the difference between their lattice energies. The detailed hydrogen bonding networks of the two polymorphs are described and compared using graph sets. Despite stabilization of the polymorphs by hydrogen bonds, pair-wise distribution function transforms show a loss of polymorphic memory upon cryogrinding the two polymorphs, leading to a difference in recrystallization behavior between amorphous piroxicam prepared from polymorphs I and II. Structural and solid-state changes of piroxicam polymorphs under mechanical stress were investigated using cryogenic grinding, PXRD, diffuse-reflectance solid-state ultraviolet-visible spectroscopy, 13C solid-state nuclear magnetic resonance spectroscopy, and diffuse-reflectance solid-state Fourier-transform infrared spectroscopy. Intermolecular proton transfer was found to accompany changes in phase and color observed upon cryogrinding the two polymorphs. Model-free and model-fitting studies of the dehydration kinetics of piroxicam monohydrate (PM) showed the dependence of activation energy ( Ea) on both isothermal and non-isothermal heating conditions, and on the fraction of conversion. In the constant-E a region, isothermal dehydration follows the two-dimensional phase boundary model, while non-isothermal dehydration follows a mechanism intermediate between two- and three-dimensional diffusion that cannot be described by any of the common models. Structural studies suggest that the complex hydrogen bond pattern in PM is responsible for the observed dehydration behavior. Ab initio calculations provide an explanation for the changes in the molecular and crystal structures accompanying the reversible change in hydration state between anhydrous piroxicam Form I and PM. The thesis further demonstrates the utility of model-free analysis in describing complex dehydration kinetics.

Physical characterization of dibasic calcium phosphate dihydrate and anhydrate.

PubMed

Miyazaki, Tamaki; Sivaprakasam, Kannan; Tantry, Jaidev; Suryanarayanan, Raj

2009-03-01

The dehydration of different commercial brands of dibasic calcium phosphate dihydrate (DCPD; CaHPO(4).2H(2)O) was examined over a range of temperatures and water vapor pressures. To determine the main factors affecting the physical stability of DCPD, the baseline characterization of DCPD and dibasic calcium phosphate anhydrate (DCPA; CaHPO(4)) was conducted by thermogravimetric analysis, differential scanning calorimetry and X-ray diffractometry. The surface area and the DCPA content (present as an impurity) depended on the commercial source of DCPD. The larger particles contained a higher concentration of DCPA and the anhydrate exhibited a concentration-dependent acceleratory effect on the dehydration of DCPD. Unlike DCPD, DCPA is physically stable and resisted hydration even when dispersed in water for over 7 months in the temperature range of 4-50 degrees C. In dosage forms containing DCPD, there is a potential for phase transformation to DCPA, while the reverse transition, that is, DCPA --> DCPD appears to be extremely unlikely. Thus, the risk of physical transformation can be minimized by using DCPA in formulations. (c) 2008 Wiley-Liss, Inc. and the American Pharmacists Association

Electrochemical properties of monolithic nickel sulfide electrodes for use in sodium batteries

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

Go, Dae-Yeon; Park, Jinsoo, E-mail: jsp@ikw.ac.kr; Noh, Pan-Jin

2014-10-15

Highlights: • We succeeded in preparing monolithic Ni{sub 3}S{sub 2} integrated electrode through the sulfuration. • The sulfuration is a facile and useful method to synthesize metal sulfides with nanostructure. • As-prepared monolithic Ni{sub 3}S{sub 2} electrodes showed very stable and cycle performance over charge/discharge cycling. - Abstract: Monolithic nickel sulfide electrodes were prepared using a facile synthesis method, sulfuration and annealing. As-prepared Ni{sub 3}S{sub 2} electrodes were characterized by X-ray diffractometry and field emission scanning electron microscopy. Thermal stability was determined by thermal gravimetric analysis and differential scanning calorimetry. Electrochemical properties were measured by galvanostatic charge and discharge cyclingmore » for Na-ion batteries. Three kinds of Ni{sub 3}S{sub 2} electrodes were prepared by varying the sulfuration time (5, 15 and 25 min). The electrochemical results indicated that the capacities increased with an increase in sulfuration time and the cycle performance was stable as a result of monolithic integration of nanostructured Ni{sub 3}S{sub 2} on Ni plates, leading to low interfacial resistance.« less

Preparation and physical properties of tara gum film reinforced with cellulose nanocrystals.

PubMed

Ma, Qianyun; Hu, Dongying; Wang, Lijuan

2016-05-01

Cellulose nanocrystals (CNC) prepared from microcrystalline cellulose were blended in tara gum solution to prepare nanocomposite films. The morphology, crystallinity, and thermal properties of the CNC and films were evaluated by using transmission electron microscopy, X-ray diffractometry, and thermogravimetric analysis, respectively. The resultant CNC was rod-shaped with diameters of around 8.6 nm. The effect of CNC content on physical and thermal properties of films was studied. The composite film tensile strength increased from 27.86 to 65.73 MPa, elastic modulus increased from 160.98 MPa to 882.49 MPa and the contact angle increased from 55.8° to 98.7° with increasing CNC content from 0 to 6 wt%. However, CNC addition increased the thermal stability slightly and CNC content above 6 wt% decreased the tensile strength by CNC aggregation in the matrix. The nanocomposite film containing 6 wt% CNC possessed the highest light transmittance, mechanical properties, and lowest oxygen permeability. CNC addition is a suitable method to modify tara gum matrix polymer properties. Copyright © 2016 Elsevier B.V. All rights reserved.