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.

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.

Study of the photovoltaic effect in thin film barium titanate

NASA Technical Reports Server (NTRS)

Grannemann, W. W.; Dharmadhikari, V. S.

1982-01-01

The basic mechanism associated with the photovoltaic phenomena observed in the R.F. sputtered BaTiO3/silicon system is presented. Series of measurements of short circuit photocurrents and open circuit photovoltage were made. The composition depth profiles and the interface characteristics of the BaTiO3/silicon system were investigated for a better understanding of the electronic properties. A Scanning Auger Microprobe combined with ion in depth profiling were used.

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

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.

The matrices of unequilibrated ordinary chondrites - Implications for the origin and history of chondrites

NASA Technical Reports Server (NTRS)

Huss, G. R.; Keil, K.; Taylor, G. J.

1981-01-01

The matrices of 16 unequilibrated chondrites were examined by optical microscopy, an electron microprobe, and a scanning electron microscope. The fine-grained, opaque, silicate matrix of type 3 unequilibrated chondrites was compositionally, mineralogically, and texturally different from the chondrules and their fragments; it may be the low temperature condensate proposed by Larimer and Anders (1967, 1970). Each meteorite has been metamorphosed by a combination of processes including thermal metamorphism and the passage of shock waves; the appearance of each chondrite results from the temperature and pressure conditions which formed it, and subsequent metamorphic alterations.

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.

Scanning proton microprobe applied to analysis of individual aerosol particles from Amazon Basin

NASA Astrophysics Data System (ADS)

Gerab, Fábio; Artaxo, Paulo; Swietlicki, Erik; Pallon, Jan

1998-03-01

The development of the Scanning Proton Microprobe (SPM) offers a new possibility for individual aerosol particle studies. The SPM joins Particle Induced X-ray Emission (PIXE) elemental analysis qualities with micrometric spatial resolution. In this work the Lund University SPM facility was used for elemental characterization of individual aerosol particles emitted to the atmosphere in the Brazilian Amazon Basin, during gold mining activities by the so-called "gold shops".

Recent advances in X-ray microanalysis in dermatology

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

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

1985-01-01

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

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.

Electron microprobe mineral analysis guide

NASA Technical Reports Server (NTRS)

Brown, R. W.

1980-01-01

Electron microprobe mineral analysis guide is a compilation of X-ray tables and spectra recorded from various mineral matrices. Spectra were obtained using electron microprobe, equipped with LiF geared, curved crystal X-ray spectrometers, utilizing typical analytical operating conditions: 15 Kv acceleration potential, 0.02 microampere sample current as measured on a clinopyroxene standard (CP19). Tables and spectra are presented for the majority of elements, fluorine through uranium, occurring in mineral samples from lunar, meteoritic and terrestrial sources. Tables for each element contain relevant analytical information, i.e., analyzing crystal, X-ray peak, background and relative intensity information, X-ray interferences and a section containing notes on the measurement. Originally intended to cover silicates and oxide minerals the tables and spectra have been expanded to cover other mineral phases. Electron microprobe mineral analysis guide is intended as a spectral base to which additional spectra can be added as the analyst encounters new mineral matrices.

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.

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

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.

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.

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

NASA Astrophysics Data System (ADS)

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

2018-07-01

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

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.

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.

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.

Study on processing immiscible materials in zero gravity

NASA Technical Reports Server (NTRS)

Reger, J. L.; Mendelson, R. A.

1975-01-01

An experimental investigation was conducted to evaluate mixing immiscible metal combinations under several process conditions. Under one-gravity, these included thermal processing, thermal plus electromagnetic mixing, and thermal plus acoustic mixing. The same process methods were applied during free fall on the MSFC drop tower facility. The design is included of drop tower apparatus to provide the electromagnetic and acoustic mixing equipment, and a thermal model was prepared to design the specimen and cooling procedure. Materials systems studied were Ca-La, Cd-Ga and Al-Bi; evaluation of the processed samples included the morphology and electronic property measurements. The morphology was developed using optical and scanning electron microscopy and microprobe analyses. Electronic property characterization of the superconducting transition temperatures were made using an impedance change-tuned coil method.

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).

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.

Determination of trace element mineral/liquid partition coefficients in melilite and diopside by ion and electron microprobe techniques

NASA Technical Reports Server (NTRS)

Kuehner, S. M.; Laughlin, J. R.; Grossman, L.; Johnson, M. L.; Burnett, D. S.

1989-01-01

The applicability of ion microprobe (IMP) for quantitative analysis of minor elements (Sr, Y, Zr, La, Sm, and Yb) in the major phases present in natural Ca-, Al-rich inclusions (CAIs) was investigated by comparing IMP results with those of an electron microprobe (EMP). Results on three trace-element-doped glasses indicated that it is not possible to obtain precise quantitative analysis by using IMP if there are large differences in SiO2 content between the standards used to derive the ion yields and the unknowns.

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.

APPLICATIONS OF CATHODOLUMINESCENCE OF QUARTZ AND FELDSPAR TO SEDIMENTARY PETROLOGY.

USGS Publications Warehouse

Ruppert, Leslie F.

1987-01-01

Cathodoluminescence (CL), the emission of visible light during electron bombardment, was first used in sandstone petrology in the mid-1960's. CL techniques are especially useful for determining the origin and source of quartz and feldspar, two of the most common constituents in clastic rocks. CL properties of both minerals are dependent on their temperature of crystallization, duration of cooling, and/or history of deformation. Detrital quartz and feldspar are typically derived from igneous and metamorphic sources and luminesce in the visible range whereas authigenic quartz and feldspar form at low temperatures and do not luminesce. Quantification of luminescent and non-luminescent quartz and feldspar with the scanning electron microscope, electron microprobe, or a commercial CL device can allow for the determination of origin, diagenesis, and source of clastic rocks when used in conjunction with field and other petrographic analyses.

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.

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.

Wavelength dispersive analysis with the synchrotron x ray fluorescence microprobe

NASA Technical Reports Server (NTRS)

Rivers, M. L.; Thorn, K. S.; Sutton, S. R.; Jones, K. W.; Bajt, S.

1993-01-01

A wavelength dispersive spectrometer (WDS) was tested on the synchrotron x ray fluorescence microprobe at Brookhaven National Laboratory. Compared to WDS spectra using an electron microprobe, the synchrotron WDS spectra have much better sensitivity and, due to the absence of bremsstrahlung radiation, lower backgrounds. The WDS spectrometer was successfully used to resolve REE L fluorescence spectra from standard glasses and transition metal K fluorescence spectra from kamacite.

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.

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.

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.

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

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.

Development of a Digital Meteorite Identification Program at University of New Mexico (UNM) (Institute of Meteoritics) and Southwestern Indian Polytechnic Institute (SIPI)

NASA Technical Reports Server (NTRS)

Gakin, R.; Lewis, K.; Simmons, J.; Gchachu, K.; Karner, J. M.; Newsom, H. E.; Jones, R. H.

2003-01-01

Determining the origin and chemical composition of suspect extra terrestrial specimens has lead to meteorite identification research programs. Such programs, like the University of New Mexico-Southwestern Indian Polytechnic Institute partnership, are being inundated with many non-meteorites (meteor wrongs) sent in by interested individuals from all over the world. This meteorite identification program developed a spreadsheet that aids in identifying the types of minerals in a sample for physical properties, possible meteorite characteristics, minerals and rock properties, and possible man made characteristics. Samples that show meteorite distinctiveness are further analyzed via the Scanning Electron Microprobe (SEM).

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.

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.

Identification of new meteorite, Mihonoseki (L), from broken fragments in Japan

NASA Technical Reports Server (NTRS)

Miura, Y.; Noma, Y.

1993-01-01

New meteorite of Mihonoseki fallen in Shimane-ken was identified by fine broken pieces by using an energy-dispersive scanning electron microprobe analyzer. It shows fusion-crust (i.e. Fe-Si melt), meteoritic minerals (kamacite, taenite, troilite, amorphous plagioclase etc.) and chrondrule with clear glassy rim. Mineralogical, and petrological data of several fine grains suggest that broken fragments of Mihonoseki are L3/4 chondritic meteorite which is the first identification in a Japanese fallen meteorite. The prompt identification method of meteorite-fragments will be applied to the next lunar, Martian and asteroid explorations, as well as meteorite falls on the terrestrial surface.

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).

Scalable hydrothermal synthesis of free-standing VO₂ nanowires in the M1 phase.

PubMed

Horrocks, Gregory A; Singh, Sujay; Likely, Maliek F; Sambandamurthy, G; Banerjee, Sarbajit

2014-09-24

VO2 nanostructures derived from solution-phase methods are often plagued by broadened and relatively diminished metal-insulator transitions and adventitious doping due to imperfect control of stoichiometry. Here, we demonstrate a stepwise scalable hydrothermal and annealing route for obtaining VO2 nanowires exhibiting almost 4 orders of magnitude abrupt (within 1 °C) metal-insulator transitions. The prepared nanowires have been characterized across their structural and electronic phase transitions using single-nanowire Raman microprobe analysis, ensemble differential scanning calorimetry, and single-nanowire electrical transport measurements. The electrical band gap is determined to be 600 meV and is consistent with the optical band gap of VO2, and the narrowness of differential scanning calorimetry profiles indicates homogeneity of stoichiometry. The preparation of high-quality free-standing nanowires exhibiting pronounced metal-insulator transitions by a solution-phase process allows for scalability, further solution-phase processing, incorporation within nanocomposites, and integration onto arbitrary substrates.

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 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.

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

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

Fabrication and surface-modification of implantable microprobes for neuroscience studies

NASA Astrophysics Data System (ADS)

Cao, H.; Nguyen, C. M.; Chiao, J. C.

2012-06-01

In this work implantable micro-probes for central nervous system (CNS) studies were developed on silicon and polyimide substrates. The probes which contained micro-electrode arrays with different surface modifications were designed for implantation in the CNS. The electrode surfaces were modified with nano-scale structures that could greatly increase the active surface area in order to enhance the electrochemical current outputs while maintaining micro-scale dimensions of the electrodes and probes. The electrodes were made of gold or platinum, and designed with different sizes. The silicon probes were modified by silicon nanowires fabricated with the vapor-liquid-solid mechanism at high temperatures. With polyimide substrates, the nanostructure modification was carried out by applying concentrated gold or silver colloid solutions onto the micro-electrodes at room temperature. The surfaces of electrodes before and after modification were observed by scanning electron microscopy. The silicon nanowire-modified surface was characterized by cyclic voltammetry. Experiments were carried out to investigate the improvement in sensing performance. The modified electrodes were tested with H2O2, electrochemical L-glutamate and dopamine. Comparisons between electrodes with and without nanostructure modification were conducted showing that the modifications have enhanced the signal outputs of the electrochemical neurotransmitter sensors.

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

Scanning dimensional measurement using laser-trapped microsphere with optical standing-wave scale

NASA Astrophysics Data System (ADS)

Michihata, Masaki; Ueda, Shin-ichi; Takahashi, Satoru; Takamasu, Kiyoshi; Takaya, Yasuhiro

2017-06-01

We propose a laser trapping-based scanning dimensional measurement method for free-form surfaces. We previously developed a laser trapping-based microprobe for three-dimensional coordinate metrology. This probe performs two types of measurements: a tactile coordinate and a scanning measurement in the same coordinate system. The proposed scanning measurement exploits optical interference. A standing-wave field is generated between the laser-trapped microsphere and the measured surface because of the interference from the retroreflected light. The standing-wave field produces an effective length scale, and the trapped microsphere acts as a sensor to read this scale. A horizontal scan of the trapped microsphere produces a phase shift of the standing wave according to the surface topography. This shift can be measured from the change in the microsphere position. The dynamics of the trapped microsphere within the standing-wave field was estimated using a harmonic model, from which the measured surface can be reconstructed. A spherical lens was measured experimentally, yielding a radius of curvature of 2.59 mm, in agreement with the nominal specification (2.60 mm). The difference between the measured points and a spherical fitted curve was 96 nm, which demonstrates the scanning function of the laser trapping-based microprobe for free-form surfaces.

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.

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

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

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

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

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.

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.

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.

Effect of LID (Registered) processing on the microstructure and mechanical properties of Ti-6Al-4V and Ti-6Al-2Sn-4Zr-2Mo titanium foil-gauge materials

NASA Technical Reports Server (NTRS)

Balckburn, Linda B.

1987-01-01

A study was undertaken to determine the mechanical properties and microstructures resulting from Liquid Interface Diffusion (LID -Registered) processing of foil-gauge specimens of Ti-6Al-4V and Ti-6Al-2Sn-4Zr-2Mo coated with varying amounts of LID material. In addition, the effects of various elevated temperature exposures on the concentration profiles of the LID alloying elements were investigated, using specimens with a narrow strip of LID material applied to the surface. Room and elevated temperature tensile properties were determined for both coated and uncoated specimens. Optical microscopy was used to examine alloy microstructures, and scanning electron microscopy to examine fracture surface morphologies. The chemical concentration profiles of the strip-coated specimens were determined with an electron microprobe.

Microchondrule-bearing clast in the Piancaldoli LL3 meteorite - A new kind of type 3 chondrite and its relevance to the history of chondrules

NASA Technical Reports Server (NTRS)

Rubin, A. E.; Scott, E. R. D.; Keil, K.

1982-01-01

Electron microprobe, scanning electron microscope, and petrographic analyses of the microchondritic clast of the Piancaldoli LL3 chondrite are reported and compared with other type three chondrites. The clast, like other type three chondrites, has a fine-grained Fe-rich opaque silicate matrix, sharply defined chondrules, abundant low-Ca clinopyroxene and minor troilite and Si and Cr-bearing metallic Fe, Ni. However, the very high model matrix abundance, unique characteristics of the chondrules, and absence of microscopically observable olivine indicate that the clast is a new type of type three chondrite. It is concluded that the microchondrules were formed by the same process that formed normal-sized chondrules in type three chondrites: melting of preexisting dustballs. It is suggested that dust grains were mineralogically sorted in the nebula before aggregating into dustballs.

Oxidation in oxygen at 900 deg and 1000 deg C of four nickel-base cast superalloys: NASA-TRW VIA, B-1900, alloy 713C, and IN-738

NASA Technical Reports Server (NTRS)

Fryburg, G. C.; Kohl, F. J.; Stearns, C. A.

1977-01-01

The oxidation at 900 and 1,000 C of four nickel-base superalloys in 1 atmosphere of slowly flowing oxygen was investigated. Thermogravimetric rate data were obtained for periods to 100 hours. The morphology and composition of the oxide scales formed after 100 hours were studied by optical microscopy, X-ray diffraction, electron microprobe, scanning electron microscopy, and X-ray photoelectron spectroscopy (ESCA). Alloys B-1900 and VIA were found to be primarily alumina formers, though probably 25 percent of their surface was covered by CR2O3-containing oxides at 900 C. Alloys 713C and IN-738 were primarily chromia formers, though the surface of 713C at 1,000 C was covered with NiO, and the surface of IN-738 at both temperatures was covered with a thin layer of TiO2.

Joining of Silicon Carbide: Diffusion Bond Optimization and Characterization

NASA Technical Reports Server (NTRS)

Halbig, Michael C.; Singh, Mrityunjay

2008-01-01

Joining and integration methods are critically needed as enabling technologies for the full utilization of advanced ceramic components in aerospace and aeronautics applications. One such application is a lean direct injector for a turbine engine to achieve low NOx emissions. In the application, several SiC substrates with different hole patterns to form fuel and combustion air channels are bonded to form the injector. Diffusion bonding is a joining approach that offers uniform bonds with high temperature capability, chemical stability, and high strength. Diffusion bonding was investigated with the aid of titanium foils and coatings as the interlayer between SiC substrates to aid bonding. The influence of such variables as interlayer type, interlayer thickness, substrate finish, and processing time were investigated. Optical microscopy, scanning electron microscopy, and electron microprobe analysis were used to characterize the bonds and to identify the reaction formed phases.

Joining of Silicon Carbide Through the Diffusion Bonding Approach

NASA Technical Reports Server (NTRS)

Halbig, Michael .; Singh, Mrityunjay

2009-01-01

In order for ceramics to be fully utilized as components for high-temperature and structural applications, joining and integration methods are needed. Such methods will allow for the fabrication the complex shapes and also allow for insertion of the ceramic component into a system that may have different adjacent materials. Monolithic silicon carbide (SiC) is a ceramic material of focus due to its high temperature strength and stability. Titanium foils were used as an interlayer to form diffusion bonds between chemical vapor deposited (CVD) SiC ceramics with the aid of hot pressing. The influence of such variables as interlayer thickness and processing time were investigated to see which conditions contributed to bonds that were well adhered and crack free. Optical microscopy, scanning electron microscopy, and electron microprobe analysis were used to characterize the bonds and to identify the reaction formed phases.

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.

Plasma sprayed coatings for containment of Cu-Mg-Si metallic phase change material

DOE PAGES

Withey, Elizabeth Ann; Kruizenga, Alan Michael; Andraka, Charles E.; ...

2016-01-01

In this study, the performance of Y 2O 3-stabilized ZrO 2 (YSZ), Y 2O 3, and Al 2O 3 plasma sprayed coatings are investigated for their ability to prevent attack of Haynes 230 by a near-eutectic Cu-Mg-Si metallic phase change material (PCM) in a closed environment at 820 °C. Areas where coatings failed were identified with optical and scanning electron microscopy, while chemical interactions were clarified through elemental mapping using electron microprobe analysis. Despite its susceptibility to reduction by Mg, the Al 2O 3 coating performed well while the YSZ and Y 2O 3 coating showed clear areas of attack.more » These results are attributed to the evolution of gaseous Mg at 820 °C leading to the formation of MgO and MgAl 2O 4.« less

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.

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.

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.

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

Scanning electron microscope and dye penetration test: comparison of root canal preparation with 15 F CO2 laser microprobe versus conventional method--in vivo study

NASA Astrophysics Data System (ADS)

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

1999-05-01

The study was conducted on 30 vital maxillary or mandibulary teeth destined for extraction due to periodontal problems. 21 were experimentally treated with pulsed CO2 laser delivered by a newly developed fiber and 9 teeth represented the control group. The micro probe is a flexible, hollow, metal fiber, 300 μm in diameter and 20 mm in length, coupled onto a handpiece, with the following radiation parameters: wavelength-10.6μm pulse duration-50m.sec; energy per pulses 0.25 joule; energy density-360 J/cm2 per pulse; power on tissue-5W. The laser group was divided into three, receiving 20, 40 or 60 pulses, respectively. On light microscopy: in all the control group cases, large amount of residual pulp tissue was seen, it was diminished in some of the low energy group and was totally eradicated in the high energy group. This was confirmed by the scanning electron microscope (SEM) examination. The dentin tubuli were partly occluded with the low energy levels and completely with the high levels, as shown by the high-speed centrifuge dye penetration test and by the SEM tests.

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.

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

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.

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.

Hot corrosion evaluation of aluminide coated superalloys in support of an ASTM Round Robin program

NASA Technical Reports Server (NTRS)

Santoro, G.

1975-01-01

Commercial aluminized coatings on substrates were hot corroded at 900 C in a 0.3 Mach burner rig with 5 ppm synthetic sea salt and at two cycling frequencies. Extensive post-exposure examinations were conducted on the corroded specimens such as metallography, X-ray diffraction, scanning electron microscopy, microprobe raster scans, and spectrographic analyses. Thermodynamic calculations were made of the equilibrium burner flame composition and the calculations were compared to the experimental findings. It was found that localized spalling of the coatings preceded coating failure. It is suggested that the spalling of the coatings is due to the formation of localized stresses caused by the depletion of chromium and aluminum in the coating or the enrichment of the coating with sulfur. For the materials and test conditions investigated, it was found that coating life is dependent only upon the initial coating thickness and not on the type of aluminized coating, the substrate, or the cycle frequency.

Nanoscale Mineralogy and Composition of Experimental Regolith Agglutinates Produced under Asteroidal Impact Conditions

NASA Technical Reports Server (NTRS)

Christoffersen, Roy; Cintala, M. J.; Keller, L. P.; See, T. H.; Horz, F.

2013-01-01

On the Moon, the energetics of smaller impactors and the physical/chemical characteristics of the granular regolith target combine to form a key product of lunar space weathering: chemically reduced shock melts containing optically-active nanophase Fe metal grains (npFe0) [1]. In addition to forming the optically dark glassy matrix phase in lunar agglutinitic soil particles [1], these shock melts are becoming increasingly recognized for their contribution to optically active patina coatings on a wide range of exposed rock and grain surfaces in the lunar regolith [2]. In applying the lessons of lunar space weathering to asteroids, the potential similarities and differences in regolith-hosted shock melts on the Moon compared to those on asteroids has become a topic of increasing interest [3,4]. In a series of impact experiments performed at velocities applicable to the asteroid belt [5], Horz et al. [6] and See and Horz [7] have previously shown that repeated impacts into a gabbroic regolith analog target can produce melt-welded grain aggregates morphologically very similar to lunar agglutinates [6,7]. Although these agglutinate-like particles were extensively analyzed by electron microprobe and scanning electron microscopy (SEM) as part of the original study [7], a microstructural and compositional comparison of these aggregates to lunar soil agglutinates at sub-micron scales has yet to be made. To close this gap, we characterized a representative set of these aggregates using a JEOL 7600 field-emission scanning electron microscope (FE-SEM), and JEOL 2500SE field-emission scanning transmission electron microscope (FE-STEM) both optimized for energy dispersive X-ray spectroscopy (EDX) compositional spectrum imaging at respective analytical spatial resolutions of 0.5 to 1 micron, and 2 to 4 nm.

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".

Ultrastructure of selected struvite-containing urinary calculi from dogs.

PubMed

Domingo-Neumann, R A; Ruby, A L; Ling, G V; Schiffman, P S; Johnson, D L

1996-09-01

To elucidate the ultrastructural details of struvite-containing urinary calculi from dogs. 38 specimens were selected from a collection of approximately 13,000 canine urinary calculi: 18 of these were composed entirely of struvite, and 20 consisted of struvite and calcium phosphate (apatite). Qualitative and quantitative analyses of specimens included use of plain and polarized light microscopy, x-ray diffractometry, scanning electron microscopy with backscattered electron imagery, x-ray fluorescence scans, and electron microprobe analysis. 4 textural types were recognized among struvite calculi, and 4 textural types of struvite-apatite calculi were described. Evidences of calculus dissolution were described from 4 calculi studied. The presence of small, well interconnected primary pores in struvite-containing urinary calculi from dogs appears to be a significant factor in determining the possible interaction of calculi with changes in the urine composition. The progress of dissolution from the calculus surface to the calculus interior appears to be largely affected by the primary porosity originally present between crystals forming the calculus framework. Apatite was observed to be more resistant to dissolution than struvite. The prevalence of fine concentric laminations having low porosity, and the common occurrence of apatite among struvite-containing urinary calculi from dogs may be 2 reasons why the efficacy of dietary and medicinal manipulations in dissolving urinary calculi is greater among cats than it is among dogs.

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.

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.

Graphene oxide windows for in situ environmental cell photoelectron spectroscopy.

PubMed

Kolmakov, Andrei; Dikin, Dmitriy A; Cote, Laura J; Huang, Jiaxing; Abyaneh, Majid Kazemian; Amati, Matteo; Gregoratti, Luca; Günther, Sebastian; Kiskinova, Maya

2011-08-28

The performance of new materials and devices often depends on processes taking place at the interface between an active solid element and the environment (such as air, water or other fluids). Understanding and controlling such interfacial processes require surface-specific spectroscopic information acquired under real-world operating conditions, which can be challenging because standard approaches such as X-ray photoelectron spectroscopy generally require high-vacuum conditions. The state-of-the-art approach to this problem relies on unique and expensive apparatus including electron analysers coupled with sophisticated differentially pumped lenses. Here, we develop a simple environmental cell with graphene oxide windows that are transparent to low-energy electrons (down to 400 eV), and demonstrate the feasibility of X-ray photoelectron spectroscopy measurements on model samples such as gold nanoparticles and aqueous salt solution placed on the back side of a window. These proof-of-principle results show the potential of using graphene oxide, graphene and other emerging ultrathin membrane windows for the fabrication of low-cost, single-use environmental cells compatible with commercial X-ray and Auger microprobes as well as scanning or transmission electron microscopes.

Silver/oxygen depth profile in coins by using laser ablation, mass quadrupole spectrometer and X-rays fluorescence

NASA Astrophysics Data System (ADS)

Cutroneo, M.; Torrisi, L.; Caridi, F.; Sayed, R.; Gentile, C.; Mondio, G.; Serafino, T.; Castrizio, E. D.

2013-05-01

Silver coins belonging to different historical periods were investigated to determine the Ag/O atomic ratio depth profiles. Laser ablation has been employed to remove, in high vacuum, the first superficial layers of the coins. Mass quadrupole spectrometry has been used to detect the Ag and the O atomic elements vaporized from the coin surface. The depth profile allowed to determine the thickness of the oxidation layer indicating that, in general, it is high in old coins. A complementary technique, using scanning electron microscope and the associated XRF microprobe, have been devoted to confirm the measurements of Ag/O atomic ratio measured with the laser-coupled mass spectrometry. The oxidation layer thicknesses range between about 25 and 250 microns.

Concrete alteration due to 55 years of exposure to river water: Chemical and mineralogical characterisation

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

Rosenqvist, Martin; Bertron, Alexandra; Fridh, Katja

This article presents a study on concrete alteration mechanisms due to 55 years of exposure to river water. Many hydro power structures in cold regions suffer from concrete deterioration at the waterline. Progressive disintegration of the concrete surface leads to exposure of the coarse aggregate and eventually the reinforcing steel. Concrete cylinders drilled out at four vertically different locations on the upstream face of a concrete dam were analysed by electron microprobe analysis, X-ray diffraction, thermogravimetry and scanning electron microscopy. Long-term exposure to the river water, which is regarded as soft water, has led to chemical and mineralogical zonation ofmore » the cement paste. Up to five zones with different chemical and mineralogical composition, parallel to the upstream face, were observed in the outermost 8–9 mm of the concrete. Decalcification, precipitation of secondary ettringite and the formation of a magnesium-rich silica gel constitute the major changes that define the zones.« less

Influence of lead ions on the macromorphology of electrodeposited zinc

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

Tsuda, Tetsuaki; Tobias, Charles W.

1981-09-01

The morphology of zinc as it is electrodeposited from acid solutions demonstrates a remarkable imprint of electrolyte flow conditions. The development of macromorphology of zinc deposits has been investigated under galvanostatic conditions on a rotating plantinum disk electrode by use of photomacrography, scanning electron microscopy, electron probe microanalysis and Auger microprobe analysis. Logarithmic spiral markings, which reflect the hydrodynamic flow on a rotating disk, appear in a certain region of current density well below the limiting current density. Morphological observations revealed the major influence of trace lead ions on the amplifications of surface roughness through coalescence and preferred growth ofmore » initial protrusions. Results obtained from ultra-pure electrolyte suggest preferred crystal growth towards well-mixed orientation in the concentration field caused by slight differences in crystallization overpotential. A qualitative model involving a coupling mechanism between the evolving surface roughness and instability phenomena in the boundary layer is advanced to explain the formation of spiral patterns.« less

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.

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.

Isomorphism and solid solutions among Ag- and Au-selenides

NASA Astrophysics Data System (ADS)

Palyanova, Galina A.; Seryotkin, Yurii V.; Kokh, Konstantin A.; Bakakin, Vladimir V.

2016-09-01

Au-Ag selenides were synthesized by heating stoichiometric mixtures of elementary substances of initial compositions Ag2-xAuxSe with a step of х=0.25 (0≤х≤2) to 1050 °С and annealing at 500 °C. Scanning electron microscopy, optical microscopy, electron microprobe analysis and X-ray powder diffraction methods have been applied to study synthesized samples. Results of studies of synthesized products revealed the existence of three solid solutions with limited isomorphism Ag↔Au: naumannite Ag2Se - Ag1.94Au0.06Se, fischesserite Ag3AuSe2 - Ag3.2Au0.8Se2 and gold selenide AuSe - Au0.94Ag0.06Se. Solid solutions and AgAuSe phases were added to the phase diagram of Ag-Au-Se system. Crystal-chemical interpretation of Ag-Au isomorphism in selenides was made on the basis of structural features of fischesserite, naumannite, and AuSe.

Analysis of ablation debris from natural and artificial iron meteorites

NASA Technical Reports Server (NTRS)

Blanchard, M. B.; Davis, A. S.

1977-01-01

Artificial ablation studies were performed on iron and nickel-iron samples using an arc-heated plasma of ionized air. Experiment conditions simulated a meteoroid traveling about 12 km/sec at an altitude of 70 km. The artificially produced fusion crusts and ablation debris show features very similar to natural fusion crusts of the iron meteorites Boguslavka, Norfork, and N'Kandhla and to magnetic spherules recovered from Mn nodules. X-ray diffraction, electron microprobe, optical, and scanning electron microscope analyses reveal that important mineralogical, elemental, and textural changes occur during ablation. Some metal is melted and ablated. The outer margin of the melted rind is oxidized and recrystallizes as a discontinuous crust of magnetite and wustite. Adjacent to the oxidized metallic ablation zone is an unoxidized metallic ablation zone in which structures such as Widmannstatten bands are obliterated as the metal is transformed to unequilibrated alpha 2 nickel-iron. Volatile elements are vaporized and less volatile elements undergo fractionation.

Large-area silicon sheet task

NASA Technical Reports Server (NTRS)

Morrison, A. D.

1982-01-01

A set of computer models was used to define a growth system configuration that was then built and used to grow web with lower thermally generated stress. Aspects of research in the edge-defined film-fed growth (EFG) method of making Si ribbon are reported. A technique was developed to determine base resistivity and carrier lifetime in semicrystalline wafers. Automated growth of 150 kg of 15 cm-dia ingot material per crucible is reviewed. Scanning transmisson electron microscopy (STEM) and microprobe investigations of processed EFG ribbon are reported. The chemical composition of the large precipitates was studied. The structural arrangement and the electrical activity of distentions or close to the central twin plane in processed material were studied. The electrical and structural properties of grain boundaries in silicon are discussed. Temperature-dependence measurements of zero-bias conductance, a photoconductivity technique, and deep-level transient spectroscopy (DLTS) were developed. A grooving and staining technique, secondary ion mass spectroscopy, and EBIC measurements in scanning electron microscopy were used to study enhanced diffusion of phosphorus at grain boundaries in polycrystaline silicon. The fundamental mechanisms of abrasion and wear and the deformation of Si by a diamond in various fluid environments are described. The efficiency of solar cells made from EFG ribbon and Semix Inc. material is reported.

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.

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

Zirconium, hafnium, and rare earth element partition coefficients for ilmenite and other minerals in high-Ti lunar mare basalts - An experimental study

NASA Technical Reports Server (NTRS)

Mckay, G.; Wagstaff, J.; Yang, S.-R.

1986-01-01

Partition coefficients were determined for Gd, Lu, Hf and Zr among ilmenite, armalcolite, and synthetic high-Ti mare basaltic melts at temperatures from 1122 deg to 1150 deg, and at oxygen fugacities of IW x 10 exp 0.5, by in situ analysis with an electron microprobe, using samples doped to present concentration levels. Coefficients for Zr were also measured for samples containing 600-1600 ppm Zr using this microprobe. In addition, coefficients were determined for Hf and Zr between chromian ulvospinel and melt, for Hf between pigeonite and melt, and for Lu between olivine and melt by microprobe analysis of samples doped to present levels. Values measured using the microprobe were in agreement with the values measured by analyzing mineral separates from the same run products by isotope dilution. Coefficient values for ilmenite are less than 0.01 for the LREE, are around 0.1 for the HREE, and are several times greater than this for Zr and Hf.

Nondestructive Testing As a Tool in the Space Shuttle Columbia Accident Investigation

NASA Technical Reports Server (NTRS)

McDanels, Steve

2008-01-01

Nondestructive testing (NDT) played a crucial role in determining the Columbia tragedy's cause. Over 84,000 pieces of debris were recovered; hundreds were subsequently subjected to NDT and materials analysis. Visual NDT of the debris revealed localized areas of damage such as erosion, excessive heating, knife edging and mechanical damage. Three-dimensional reconstructions were made of the left wing leading edge, utilizing a tripod-mounted laser scanning head and focused laser beam, and an advanced topometric optical scanner (ATOS) with digital white light to scan complex-shaped debris, producing monochrome 3-D models. Texture mapping provided a means to capture true colors of the debris and superimpose them on the scanned images. Uniform deposits were found over large portions of debris, obscuring underlying materials. To determine what was beneath, inverse radiography was enlisted. The radiographs guided investigators to where samples should be taken. To ascertain compositions, these samples were subjected to analytical testing, including energy dispersive X-ray spectroscopy and electron microprobe analysis. This combination of visual evidence, radiography, virtual reconstruction, and materials analysis allowed the forensic scientists to verify that a breach occurred in the leading edge of the left wing, the path the plasma followed, and the sequence of events that led to the loss.

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.

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

Phase state of a Bi-43 wt % Sn superplastic alloy and its changes under the effect of external mechanical stresses and aging

NASA Astrophysics Data System (ADS)

Korshak, V. F.; Chushkina, R. A.; Shapovalov, Yu. A.; Mateichenko, P. V.

2011-07-01

Samples of a Bi-43 wt % Sn superplastic alloy have been studied by X-ray diffraction in the ascast state, after compression of as-cast samples to ˜70% on a hydraulic press, after aging in the as-cast and preliminarily compressed state, and using samples deformed under superplastic conditions. The X-ray diffraction studies have been carried out using a DRON-2.0 diffractometer in Cu Kα radiation. The samples aged and deformed under superplasticity conditions have been studied using electron-microprobe analysis in a JSM-820 scanning electron microscope equipped with a LINK AN/85S EDX system. It has been found that the initial structural-phase state of the alloy was amorphous-crystalline. Causes that lead to a change in this state upon deformation and aging are discussed. A conclusion is made that the superplasticity effect manifests itself against the background of processes that are stipulated by the tendency of the initially metastable alloy to phase equilibrium similarly to what is observed in the Sn-38 wt % Pb eutectic alloy studied earlier.

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.

Elemental and topographical imaging of microscopic variations in deposition on NSTX-U and DIII-D samples

NASA Astrophysics Data System (ADS)

Skinner, C. H.; Kaita, R.; Koel, B. E.; Chrobak, C. P.; Wampler, W. R.

2017-10-01

Tokamak plasma facing components (PFCs) have surface roughness that can cause microscopic spatial variations in erosion and deposition and hence influence material migration. Previous RBS measurements showed indirect evidence for this but the spatial (0.5mm) resolution was insufficient for direct imaging. We will present elemental images at sub-micron resolution of deposition on NSTX-U and DiMES samples that show strong microscopic variations and correlate this with 3D topographical maps of surface irregularities. The elemental imaging is performed with a Scanning Auger Microprobe (SAM) that measures element-specific Auger electrons excited by an SEM electron beam. 3D topographical maps of the samples are performed with a Leica DCM 3D confocal light microscope and compared to the elemental deposition pattern. The initial results appear consistent with erosion at the downstream edges of the surface pores exposed to the incident ion flux, whereas the deeper regions are shadowed and serve as deposition traps. Support was provided through DOE Contract Numbers DE-AC02-09CH11466, DE-FC02-04ER54698 and DE-NA0003525.

The effect of silicon on the interaction between metallic uranium and aluminum: A 50 year long diffusion experiment

NASA Astrophysics Data System (ADS)

Leenaers, A.; Detavernier, C.; Van den Berghe, S.

2008-11-01

The core of the BR1 research reactor at SCK•CEN, Mol (Belgium) has a graphite matrix loaded with fuel rods consisting of a natural uranium slug in aluminum cladding. The BR1 reactor has been in operation since 1956 and still contains its original fuel rods. After more than 50 years irradiation at low temperature, some of the fuel rods have been examined. Fabrication reports indicate that a so-called AlSi bonding layer and an U(Al,Si) 3 anti-diffusion layer on the natural uranium fuel slug were applied to limit the interaction between the uranium fuel and aluminum cladding. The microstructure of the fuel, bonding and anti-diffusion layer and cladding were analysed using optical microscopy, scanning electron microscopy and electron microprobe analysis. It was found that the AlSi bonding layer does provide a tight bond between fuel and cladding but that it is a thin USi layer that acts as effective anti-diffusion layer and not the intended U(Al,Si) 3 layer.

Geochemical and mineralogical controls on metal(loid) mobility in the oxide zone of the Prairie Creek Deposit, NWT

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

Stavinga, Drew; Jamieson, Heather; Layton-Matthews, Daniel

2017-02-01

Prairie Creek is an unmined high grade Zn-Pb-Ag deposit in the southern Mackenzie Mountains of the Northwest Territories, located in a 320 km2 enclave surrounded by the Nahanni National Park reserve. The upper portion of the quartz-carbonate-sulphide vein mineralization has undergone extensive oxidation, forming high grade zones, rich in smithsonite (ZnCO3) and cerussite (PbCO3). This weathered zone represents a significant resource and a potential component of mine waste material. This study is focused on characterizing the geochemical and mineralogical controls on metal(loid) mobility under mine waste conditions, with particular attention to the metal carbonates as a potential source of tracemore » elements to the environment. Analyses were conducted using a combination of microanalytical techniques (electron microprobe, scanning electron microscopy with automated mineralogy, laser-ablation inductively-coupled mass spectrometry, and synchrotron-based element mapping, micro-X-ray diffraction and micro-X-ray absorbance). The elements of interest included Zn, Pb, Ag, As, Cd, Cu, Hg, Sb and Se.« less

Trace elements in hydrothermal quartz: Relationships to cathodoluminescent textures and insights into vein formation

USGS Publications Warehouse

Rusk, B.G.; Lowers, H.A.; Reed, M.H.

2008-01-01

High-resolution electron microprobe maps show the distribution of Ti, Al, Ca, K, and Fe among quartz growth zones revealed by scanning electron microscope-cathodoluminescence (SEM-CL) from 12 hydrothermal ore deposits formed between ???100 and e1750 ??C. The maps clearly show the relationships between trace elements and CL intensity in quartz. Among all samples, no single trace element consistently correlates with variations in CL intensity. However in vein quartz from five porphyry-Cu (Mo-Au) deposits, CL intensity always correlates positively with Ti concentrations, suggesting that Ti is a CL activator in quartz formed at >400 ??C. Ti concentrations in most rutile-bearing vein quartz from porphyry copper deposits indicate reasonable formation temperatures of 2000 ppm, but in high-temperature quartz, Al concentrations are consistently in the range of several hundred ppm. Aluminum concentrations in quartz refl ect the Al solubility in hydrothermal fluids, which is strongly dependent on pH. Aluminum concentrations in quartz therefore reflect fluctuations in pH that may drive metal-sulfide precipitation in hydrothermal systems. ?? 2008 The Geological Society of America.

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.

Ultrastructural properties of laser-irradiated and heat-treated dentin.

PubMed

Rohanizadeh, R; LeGeros, R Z; Fan, D; Jean, A; Daculsi, G

1999-12-01

Previous studies using scanning electron microscopy and infrared absorption spectroscopy reported that laser irradiation causes compositional changes in enamel. The purpose of this study was to evaluate the ultrastructural and compositional changes in dentin caused by irradiation with a short-pulse laser (Q-switched Nd:YAG). The irradiated and non-irradiated areas of the lased dentin samples were investigated by scanning (SEM) and transmission electron microscopy (TEM), micro-micro electron diffraction, and electron microprobe analysis of dispersive energy (EDX). Heat-treated dentin was similarly investigated. This study demonstrated that laser irradiation resulted in the recrystallization of dentin apatite and in the formation of additional calcium phosphate phases consisting of magnesium-substituted beta-tricalcium phosphate, beta-TCMP, beta-(Ca,Mg)3(PO4)2, and tetracalcium phosphate, TetCP, Ca4(PO4)O. TEM analyses of the modified and unmodified zones of the irradiated areas showed two types of crystal populations: much larger crystals from the modified zone and crystals with size and morphology similar to those of dentin apatite in the unmodified zone. The morphology of crystals in the modified zones in the irradiated dentin resembled those of dentin sintered at 800 or 950 degrees C. In the irradiated areas (modified and unmodified zones), the Ca/P ratio was lower compared with that in the non-irradiated dentin. The Mg/Ca ratio in the modified zones was higher than that in the unmodified zones and in the non-irradiated dentin. In sintered dentin, the Mg/Ca ratio increased as a function of sintering temperature. The ultrastructural and compositional changes observed in laser-irradiated dentin may be attributed to high temperature and high pressure induced by microplasma during laser irradiation. These changes may alter the solubility of the irradiated dentin, making it less susceptible to acid dissolution or to the caries process.

Examination of UC-ZrC after long term irradiation at thermionic temperature

NASA Technical Reports Server (NTRS)

Yang, L.; Johnson, H. O.

1972-01-01

Two fluoride tungsten clad UC-ZrC fueled capsules, designated as V-2C and V-2D, were examined a hot cell after irradiation in NASA Plum Brook Reactor at a maximum cladding temperature of 1930 K for 11,089 and 12,031 hours to burnups of 3.0 x 10 to the 20th power and 2.1 x 10 to the 20th power fission/c.c. respectively. Percentage of fission gas release from the fuel material was measured by radiochemical means. Cladding deformation, fuel-cladding interaction and microstructures of fuel, cladding, and fuel-cladding interface were studied metallographically. Compositions of dispersions in fuel, fuel matrix and fuel-cladding interaction layer were analyzed by electron microprobe techniques. Axial and radial distributions of burnup were determined by gamma-scan, autoradiography and isotopic burnup analysis. The results are presented and discussed in conjunction with the requirements of thermionic fuel elements for space power application.

Deposit formation in hydrocarbon rocket fuels with an evaluation of a propane heat transfer correlation

NASA Technical Reports Server (NTRS)

Masters, P. A.; Aukerman, C. A.

1982-01-01

A high pressure fuel coking testing apparatus was designed and developed and was used to evaluate thermal decomposition limits and carbon decomposition rates in heated copper tubes for hydrocarbon fuels. A commercial propane (90% grade) and chemically pure (CP) propane were tested. Heat transfer to supercritical propane was evaluated at 136 atm, bulk fluid velocities of 6 to 30 m/s, and tube wall temperatures in the range of 422 to 811 K. A forced convection heat transfer correlation developed in a previous test effort verified a prediction of most of the experimental data within a + or - 30% range, with good agreement for the CP propane data. No significant differences were apparent in the predictions derived from the correlation when the carbon resistance was included with the film resistance. A post-test scanning electron microprobe analysis indicated occurrences of migration and interdiffusion of copper into the carbon deposit.

Wear and Reactivity Studies of Melt infiltrated Ceramic Matrix Composite

NASA Technical Reports Server (NTRS)

Jarmon, David C.; Ojard, Greg; Brewer, David N.

2013-01-01

As interest grows in the use of ceramic matrix composites (CMCs) for critical gas turbine engine components, the effects of the CMCs interaction with the adjoining structure needs to be understood. A series of CMC/material couples were wear tested in a custom elevated temperature test rig and tested as diffusion couples, to identify interactions. Specifically, melt infiltrated silicon carbide/silicon carbide (MI SiC/SiC) CMC was tested in combination with a nickel-based super alloy, Waspaloy, a thermal barrier coating, Yttria Stabilized Zirconia (YSZ), and a monolithic ceramic, silicon nitride (Si3N4). To make the tests more representative of actual hardware, the surface of the CMC was kept in the as-received state (not machined) with the full surface features/roughness present. Test results include: scanning electron microscope characterization of the surfaces, micro-structural characterization, and microprobe analysis.

Les fards rouges cosmétiques et rituels a base de cinabre et d'ocre de l'époque punique en Tunisie: analyse, identification et caractérisation.

PubMed

Alatrache, A; Mahjoub, H; Ayed, N; Ben Younes, H

2001-10-01

Natural antique colorants include mainly red pigments such as cinnabar and ochre. These archeological pigments were used especially as funeral and cosmetic makeup and are a material proof of handicraft activities and exchanges. The identification and characterization of a group of punic colorants, corresponding to samples discovered during excavations at several Tunisian archeological sites (Cartage, Ksour Essef, Kerkouane, Bekalta, Makthar, Bou Arada), were conducted using the least destructive analysis techniques such us scanning electron microscopy coupled to X-ray fluorescence microprobe, direct current plasma emission spectroscopy, atomic absorption spectrometry, Fourier transform infrared spectrometry and X-ray diffraction. Eleven natural red colorants from punic period were subject to this investigation and were compared to contemporary substances. Five colorants were cinnabar and the other six were ochre.

Proton-beam writing channel based on an electrostatic accelerator

NASA Astrophysics Data System (ADS)

Lapin, A. S.; Rebrov, V. A.; Kolin'ko, S. V.; Salivon, V. F.; Ponomarev, A. G.

2016-09-01

We have described the structure of the proton-beam writing channel as a continuation of a nuclear scanning microprobe channel. The problem of the accuracy of positioning a probe by constructing a new high-frequency electrostatic scanning system has been solved. Special attention has been paid to designing the probe-forming system and its various configurations have been considered. The probe-forming system that best corresponds to the conditions of the lithographic process has been found based on solving the problem of optimizing proton beam formation. A system for controlling beam scanning using multifunctional module of integrated programmable logic systems has been developed.

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.

Scanning Probe Investigation of Pitting Corrosion on Aluminum 5083 H131

DTIC Science & Technology

2014-05-01

245–254. 10. Dolic, N.; Malina, J.; Begic Hadzipasic, A. Pit Nucleation on As-Cast Aluminum Alloy AW-5083 in 0.01M NaCl. Journal of Mining and...R. A.; Stratmann, M. Application of a Kelvin Microprobe to the Corrosion in Humid Atmospheres. J. Electrochem Soc. 1991, 138 (1), 55–61. 15

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)

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.

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.

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.

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.

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

Evidence for Microfossils in Ancient Rocks and Meteorites

NASA Technical Reports Server (NTRS)

Hoover, Richard B.; Rozanov, A. Y.; Zhmur, S. I.; Gorlenko, V. M.

1998-01-01

The McKay et all. detection of chemical biomarkers and possible microfossils in an ancient meteorite from Mars (ALH84001) stimulated research in several areas of importance to the newly emerging field of Astrobiology. Their report resulted in a search for additional evidence of microfossils in ancient terrestrial rocks and meteorites. These studies of ancient rocks and meteorites were conducted independently (and later collaboratively) in the United States and Russia using the SEM, Environmental Scanning Electron Microscope (ESEM), and Field Emission Scanning Electron Microscope (FESEM). We have encountered in-situ in freshly broken carbonaceous chondrites a large number of complex microstructures that appear to be lithified microbial forms. The meteoritic microstructures have characteristics similar to the lithified remains of filamentous cyanobacteria and bacterial microfossils we have found in ancient phosphorites, ancient graphites and oil shales. Energy Dispersive Spectroscopy (EDS) and Link microprobe analysis shows the possible microfossils have a distribution of chemical elements characteristic of the meteorite rock matrix, although many exhibit a superimposed carbon enhancement. We have concluded that the mineralized bodies encountered embedded in the rock matrix of freshly fractured meteoritic surfaces can not be dismissed as recent surface contaminants. Many of the forms found in-situ in the Murchison, Efremovka, and Orgueil carbonaceous meteorites are strikingly similar to microfossils of coccoid bacteria, cyanobacteria and fungi such as we have found in the Cambrian phosphorites of Khubsugul, Mongolia and high carbon Phanerozoic and Precambrian rocks of the Siberian and Russian Platforms.

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.

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.

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.

Zirconolites from Sri Lanka, South Africa and Brazil

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

Ewing, R.C.; Haaker, R.F.; Headley, T.J.

1981-01-01

Zirconolites, CaZrTi/sub 2/O/sub 7/, from Sri Lanka and Pala Bora, South Africa, and a calzirtite, CaZr/sub 3/TiO/sub 9/, from Jacupiranga, Brazil, were examined using the electron microprobe, x-ray diffraction (annealing study), transmission electron microscopy, scanning electron microscopy and optical microscopy. The x-ray data indicate that all three zirconolites are metamict. Both Sri Lanka zirconolites are amorphous to the limits of resolution of the electron microscope (approx. 10 A). The Pala Bora zirconolite is largely amorphous but contains isolated domains (50 to 200 A) of crystalline material which may be the result of post-metamict recrystallization and alteration. The only other significantmore » evidence for chemical alteration was the lower ThO/sub 2/ concentration (1 to 2 weight percent) and slightly lower analytic totals for the rims of the Sri Lanka zirconolites. Upon annealing at 1130/sup 0/C for 5 hours, all three zirconolites recrystallized as microcrystalline aggregates. Refined unit cell parameters and volumes are consistent with published data for synthetic zirconolites. Both Sri Lanka zirconolites contain microvoids, spherical in shape, and 200 Angstroms to 2 microns in size. This porosity may be the result of helium accumulation arising from the decay of U and Th. The calzirtite was highly crystalline, exhibited no porosity, and was unchanged by the annealing treatment.« less

Heterogeneous arsenic enrichment in meta-sedimentary rocks in central Maine, United States.

PubMed

O'Shea, Beth; Stransky, Megan; Leitheiser, Sara; Brock, Patrick; Marvinney, Robert G; Zheng, Yan

2015-02-01

Arsenic is enriched up to 28 times the average crustal abundance of 4.8 mg kg(-1) for meta-sedimentary rocks of two adjacent formations in central Maine, USA where groundwater in the bedrock aquifer frequently contains elevated As levels. The Waterville Formation contains higher arsenic concentrations (mean As 32.9 mg kg(-1), median 12.1 mg kg(-1), n=38) than the neighboring Vassalboro Group (mean As 19.1 mg kg(-1), median 6.0 mg kg(-1), n=38). The Waterville Formation is a pelitic meta-sedimentary unit with abundant pyrite either visible or observed by scanning electron microprobe. Concentrations of As and S are strongly correlated (r=0.88, p<0.05) in the low grade phyllite rocks, and arsenic is detected up to 1944 mg kg(-1) in pyrite measured by electron microprobe. In contrast, statistically significant (p<0.05) correlations between concentrations of As and S are absent in the calcareous meta-sediments of the Vassalboro Group, consistent with the absence of arsenic-rich pyrite in the protolith. Metamorphism converts the arsenic-rich pyrite to arsenic-poor pyrrhotite (mean As 1 mg kg(-1), n=15) during de-sulfidation reactions: the resulting metamorphic rocks contain arsenic but little or no sulfur indicating that the arsenic is now in new mineral hosts. Secondary weathering products such as iron oxides may host As, yet the geochemical methods employed (oxidative and reductive leaching) do not conclusively indicate that arsenic is associated only with these. Instead, silicate minerals such as biotite and garnet are present in metamorphic zones where arsenic is enriched (up to 130.8 mg kg(-1) As) where S is 0%. Redistribution of already variable As in the protolith during metamorphism and contemporary water-rock interaction in the aquifers, all combine to contribute to a spatially heterogeneous groundwater arsenic distribution in bedrock aquifers. Copyright © 2014 Elsevier B.V. All rights reserved.

Biologic Rhythms Derived from Siberian Mammoths' Hairs

PubMed Central

Spilde, Mike; Lanzirotti, Antonio; Qualls, Clifford; Phillips, Genevieve; Ali, Abdul-Mehdi; Agenbroad, Larry; Appenzeller, Otto

2011-01-01

Hair is preserved for millennia in permafrost; it enshrines a record of biologic rhythms and offers a glimpse at chronobiology as it was in extinct animals. Here we compare biologic rhythms gleaned from mammoth's hairs with those of modern human hair. Four mammoths' hairs came from varying locations in Siberia 4600 km, four time zones, apart ranging in age between 18,000 and 20,000 years before present. We used two contemporaneous human hairs for comparison. Power spectra derived from hydrogen isotope ratios along the length of the hairs gave insight into biologic rhythms, which were different in the mammoths depending on location and differed from humans. Hair growth for mammoths was ∼31 cms/year and ∼16 cms/year for humans. Recurrent annual rhythms of slow and fast growth varying from 3.4 weeks/cycles to 8.7 weeks/cycles for slow periods and 1.2 weeks/cycles to 2.2 weeks/cycles for fast periods were identified in mammoth's hairs. The mineral content of mammoth's hairs was measured by electron microprobe analysis (k-ratios), which showed no differences in sulfur amongst the mammoth hairs but significantly more iron then in human hair. The fractal nature of the data derived from the hairs became evident in Mandelbrot sets derived from hydrogen isotope ratios, mineral content and geographic location. Confocal microscopy and scanning electron microscopy showed varied degrees of preservation of the cuticle largely independent of age but not location of the specimens. X-ray fluorescence microprobe and fluorescence computed micro-tomography analyses allowed evaluation of metal distribution and visualization of hollow tubes in the mammoth's hairs. Seasonal variations in iron and copper content combined with spectral analyses gave insights into variation in food intake of the animals. Biologic rhythms gleaned from power spectral plots obtained by modern methods revealed life style and behavior of extinct mega-fauna. PMID:21747920

Heterogeneous arsenic enrichment in meta-sedimentary rocks in central Maine, United States

PubMed Central

O’Shea, Beth; Stransky, Megan; Leitheiser, Sara; Brock, Patrick; Marvinney, Robert G.; Zheng, Yan

2014-01-01

Arsenic is enriched up to 28 times the average crustal abundance of 4.8 mg kg−1 for meta-sedimentary rocks of two adjacent formations in central Maine, USA where groundwater in the bedrock aquifer frequently contains elevated As levels. The Waterville Formation contains higher arsenic concentrations (mean As 32.9 mg kg−1, median 12.1 mg kg−1, n=36) than the neighboring Vassalboro Group (mean As 19.1 mg kg−1, median 6.0 mg kg−1, n=36). The Waterville Formation is a pelitic meta-sedimentary unit with abundant pyrite either visible or observed by scanning electron microprobe. Concentrations of As and S are strongly correlated (r=0.88, p<0.05) in the low grade phyllite rocks, and arsenic is detected up to 1,944 mg kg−1 in pyrite measured by electron microprobe. In contrast, statistically significant (p<0.05) correlations between concentrations of As and S are absent in the calcareous meta-sediments of the Vassalboro Group, consistent with the absence of arsenic-rich pyrite in the protolith. Metamorphism converts the arsenic-rich pyrite to arsenic-poor pyrrhotite (mean As 1 mg kg−1, n=15) during de-sulfidation reactions: the resulting metamorphic rocks contain arsenic but little or no sulfur indicating that the arsenic is now in new mineral hosts. Secondary weathering products such as iron oxides may host As, yet the geochemical methods employed (oxidative and reductive leaching) do not conclusively indicate that arsenic is associated only with these. Instead, silicate minerals such as biotite and garnet are present in metamorphic zones where arsenic is enriched (up to 130.8 mg kg−1 As) where S is 0%. Redistribution of already variable As in the protolith during metamorphism and contemporary water-rock interaction in the aquifers, all combine to contribute to a spatially heterogeneous groundwater arsenic distribution in bedrock aquifers. PMID:24861530

Sub-Micrometer Scale Minor Element Mapping in Interplanetary Dust Particles: A Test for Stratospheric Contamination

NASA Technical Reports Server (NTRS)

Flynn, G. J.; Keller, L. P.; Sutton, S. R.

2004-01-01

Combined X-ray microprobe (XRM), energy dispersive x-ray fluorescence using a Transmission Electron Microscope (TEM), and electron microprobe measurements have determined that the average bulk chemical composition of the interplanetary dust particles (IDPs) collected from the Earth s stratosphere is enriched relative to the CI meteorite composition by a factor of 2 to 4 for carbon and for the moderately volatile elements Na, K, P, Mn, Cu, Zn, Ga, Ge, and Se, and enriched to approximately 30 times CI for Br. However, Jessberger et al., who have reported similar bulk enrichments using Proton Induced X-ray Emission (PIXE), attribute the enrichments to contamination by meteor-derived atmospheric aerosols during the several weeks these IDPs reside in the Earth s atmosphere prior to collection. Using scanning Auger spectroscopy, a very sensitive surface analysis technique, Mackinnon and Mogk have observed S contamination on the surface of IDPs, presumably due to the accretion of sulfate aerosols during stratospheric residence. But the S-rich layer they detected was so thin (approximately 100 angstroms thick) that the total amount of S on the surface was too small to significantly perturb the bulk S-content of a chondritic IDP. Stephan et al. provide support for the contamination hypothesis by reporting the enrichment of Br on the edges of the IDPs using Time-of-Flight Secondary-Ion Mass-Spectrometry (TOFSIMS), but TOF-SIMS is notorious for producing false edge-effects, particularly on irregularly-shaped samples like IDPs. Sutton et al. mapped the spatial distribution of Fe, Ni, Zn, Br, and Sr, at the approximately 2 m scale, in four IDPs using element-specific x-ray fluorescence (XRF) computed microtomography. They found the moderately volatile elements Zn and Br, although spatially inhomogeneous, were not concentrated on the surface of any of the IDPs they examined, suggesting that the Zn and the Br enrichments in the IDPs are not due to contamination during stratospheric residence.

Biologic Rhythms Derived from Siberian Mammoths Hairs

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

M Spilde; A Lanzirotti; C Qualls

2011-12-31

Hair is preserved for millennia in permafrost; it enshrines a record of biologic rhythms and offers a glimpse at chronobiology as it was in extinct animals. Here we compare biologic rhythms gleaned from mammoth's hairs with those of modern human hair. Four mammoths' hairs came from varying locations in Siberia 4600 km, four time zones, apart ranging in age between 18,000 and 20,000 years before present. We used two contemporaneous human hairs for comparison. Power spectra derived from hydrogen isotope ratios along the length of the hairs gave insight into biologic rhythms, which were different in the mammoths depending onmore » location and differed from humans. Hair growth for mammoths was {approx}31 cms/year and {approx}16 cms/year for humans. Recurrent annual rhythms of slow and fast growth varying from 3.4 weeks/cycles to 8.7 weeks/cycles for slow periods and 1.2 weeks/cycles to 2.2 weeks/cycles for fast periods were identified in mammoth's hairs. The mineral content of mammoth's hairs was measured by electron microprobe analysis (k-ratios), which showed no differences in sulfur amongst the mammoth hairs but significantly more iron then in human hair. The fractal nature of the data derived from the hairs became evident in Mandelbrot sets derived from hydrogen isotope ratios, mineral content and geographic location. Confocal microscopy and scanning electron microscopy showed varied degrees of preservation of the cuticle largely independent of age but not location of the specimens. X-ray fluorescence microprobe and fluorescence computed micro-tomography analyses allowed evaluation of metal distribution and visualization of hollow tubes in the mammoth's hairs. Seasonal variations in iron and copper content combined with spectral analyses gave insights into variation in food intake of the animals. Biologic rhythms gleaned from power spectral plots obtained by modern methods revealed life style and behavior of extinct mega-fauna.« less

Biologic rhythms derived from Siberian mammoths' hairs.

PubMed

Spilde, Mike; Lanzirotti, Antonio; Qualls, Clifford; Phillips, Genevieve; Ali, Abdul-Mehdi; Agenbroad, Larry; Appenzeller, Otto

2011-01-01

Hair is preserved for millennia in permafrost; it enshrines a record of biologic rhythms and offers a glimpse at chronobiology as it was in extinct animals. Here we compare biologic rhythms gleaned from mammoth's hairs with those of modern human hair. Four mammoths' hairs came from varying locations in Siberia 4600 km, four time zones, apart ranging in age between 18,000 and 20,000 years before present. We used two contemporaneous human hairs for comparison. Power spectra derived from hydrogen isotope ratios along the length of the hairs gave insight into biologic rhythms, which were different in the mammoths depending on location and differed from humans. Hair growth for mammoths was ∼31 cms/year and ∼16 cms/year for humans. Recurrent annual rhythms of slow and fast growth varying from 3.4 weeks/cycles to 8.7 weeks/cycles for slow periods and 1.2 weeks/cycles to 2.2 weeks/cycles for fast periods were identified in mammoth's hairs. The mineral content of mammoth's hairs was measured by electron microprobe analysis (k-ratios), which showed no differences in sulfur amongst the mammoth hairs but significantly more iron then in human hair. The fractal nature of the data derived from the hairs became evident in Mandelbrot sets derived from hydrogen isotope ratios, mineral content and geographic location. Confocal microscopy and scanning electron microscopy showed varied degrees of preservation of the cuticle largely independent of age but not location of the specimens. X-ray fluorescence microprobe and fluorescence computed micro-tomography analyses allowed evaluation of metal distribution and visualization of hollow tubes in the mammoth's hairs. Seasonal variations in iron and copper content combined with spectral analyses gave insights into variation in food intake of the animals. Biologic rhythms gleaned from power spectral plots obtained by modern methods revealed life style and behavior of extinct mega-fauna.

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.

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.

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.

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.

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.

Hot Corrosion Degradation of Metals and Alloys - A Unified Theory

DTIC Science & Technology

1979-06-01

microscope, electron beam microprobe and X-ray diffraction. REULTS AND DMCtESION Hot Corrosion Degradation Sectuence In attempting to develop a unified...Figure 40a. Such ghost images, which can be called corrosion front ghosts , appear as sequential dark and light zones in electron backscatter images... Electronic and Solid State Sciences AUG Ill 1979I Bolling AFB, D.C. 20332 ID PRATT &WHITNEY ARCRAFT GROUP P.O . Box 2861 /Government Products Division wi

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

Chambers, W.F.; Doyle, J.H.

QUANT is a special schedule for electron microprobes which are automated with Tracor Northern electronics. QUANT is called from the SANDIA TASK-78 control program and provides simultaneous data acquisition and data reduction capabilities using either a first principles atomic number, absorption, fluorescence (ZAF) technique or a matrix correction (Bence--Albee) technique. During operation, QUANT controls the execution of three auxiliary programs - BA78, ZAF78, and SETUP.

Use of geochemical mass balance modelling to evaluate the role of weathering in determining stream chemistry in five mid-Atlantic watersheds on different lithologies

USGS Publications Warehouse

O'Brien, Anne K.; Rice, Karen C.; Bricker, Owen P.; Kennedy, Margaret M.; Anderson, R. Todd

1997-01-01

The importance of mineral weathering was assessed and compared for five mid-Atlantic watersheds receiving similar atmospheric inputs but underlain by differing bedrock. Annual solute mass balances and volume-weighted mean solute concentrations were calculated for each watershed for each year of record. In addition, primary and secondary mineralogy were determined for each of the watersheds through analysis of soil samples and thin sections using petrographic, scanning electron microscope, electron microprobe and X-ray diffraction techniques. Mineralogical data were also compiled from the literature. These data were input to NETPATH, a geochemical program that calculates the masses of minerals that react with precipitation to produce stream water chemistry. The feasibilities of the weathering scenarios calculated by NETPATH were evaluated based on relative abundances and reactivities of minerals in the watershed. In watersheds underlain by reactive bedrocks, weathering reactions explained the stream base cation loading. In the acid-sensitive watersheds on unreactive bedrock, calculated weathering scenarios were not consistent with the abundance of reactive minerals in the underlying bedrock, and alternative sources of base cations are discussed.

An unusual occurrence of arsenic-bearing pyrite in the Upper Freeport coal bed, West-Central Pennsylvania

USGS Publications Warehouse

Ruppert, L.F.; Minkin, J.A.; McGee, J.J.; Cecil, C.B.

1992-01-01

Scanning electron microscopy and electron microprobe analysis were used to identify a rare type of As-bearing pyrite in selected specific gravity separates from the Pennsylvanian age Upper Freeport coal bed, west-central Pennsylvania. Arsenic was detected mainly in cell-wall replacement pyrite where concentrations ranged from nondetectable to 1.9 wt %. Although the majority of arsenic-bearing pyrite in the Upper Freeport coal bed is concentrated in massive and late diagenetic pyrite morphologies, the rarer As-bearing cell-replacement pyrite was observed in both light and heavy gravity separates from the three coal facies examined. Arsenic was occasionally detected in cell-filling replacement pyrite, but this As appears to be an artifact produced by signals from underlying and/or adjacent As-bearing cell-wall replacement pyrite. It is postulated that some plants of the Upper Freeport paleoswamp may have biomethylated As, which later could have been converted to dimethylarsine or other volatile organoarsenic compounds by either biologically or chemically driven processes. Once liberated, the arsenic may have been incorporated into pyrite during pyritization of the cell walls. The As incorporation occurred early, before significant compaction of the peat, because the pyritized cell walls are not compacted.

Attenuation of heavy metals by geosynthetics in the coal gangue-filled columns.

PubMed

Wang, Ping; Hu, Zhenqi; Wang, Peijun

2013-01-01

In the subsided areas backfilled with coal gangue, an issue of continuing environmental concern is the migration of hazardous metals to the subsurface soil and groundwater. As an effective isolation material, geosynthetics have been scarcely applied into mining areas reclamation of China. This paper describes research aimed at characterizing the behaviours of different geosynthetics in the leaching columns filled with coal gangues. Four types of geosynthetics were selected: fibres needle-punched nonwoven geotextiles, high-density polyethylene, needle-punched Na-bentonite geosynthetic clay liner (GCL-NP) and Na-bentonite geosynthetic-overbited film. Heavy metals were significantly attenuated and by monitoring aqueous solutions in the whole percolation period, negative correlation was found between pH value and concentration of heavy metals. Generally, GCL-NP showed comparatively better effects on attenuating the migration of heavy metals. According to the meta-analysis of heavy metals present in the leachates and retained in the columns, geosynthetics have good capabilities of sorption and retardation, which can delay the breakthrough time of heavy metals and retard the accumulation in the subsurface. Future research will use X-ray diffraction and micro-imaging (electron microprobe and scanning electron microscopy) to further explain retention mechanisms.

Mineralogy, textures and mode of formation of a hibonite-bearing Allende inclusion

NASA Technical Reports Server (NTRS)

Allen, J. M.; Grossman, L.; Davis, A. M.; Hutcheon, I. D.

1978-01-01

The origin of a Type A, hibonite-rich, coarse-grained inclusion is investigated with the electron microprobe and petrographic and scanning electron microscopes. The primary phases are hibonite, rhonite, Ti-Al-pyroxene, spinel, perovskite and melilite. Evidence for the crystallization of the bulk of the primary phases, hibonite and melilite, from a melt is lacking, suggesting that they may have condensed directly from a solar nebular gas instead. Primary phases were intensely altered during a later condensation event which deposited grossular, anorthite, nepheline and wollastonite in veins and cavities. Four or five condensate rims were deposited as successive layers on the outside of the inclusion. From inside to outside, they consist of perovskite + spinel, nepheline + anorthite, Ti-Al-pyroxene + diopside, hedenbergite + or - wollastonite + or - andradite and, finally, prisms of diopside and hedenbergite with wollastonite and andradite. Reverse zoning in melilite; alteration phases and rim phases, which are not stable condensates from a gas of solar composition; and details of the sequence of rim condensates all suggest that the entire condensation history of this inclusion was interrupted by changes in pressure and/or temperature and/or gas phase composition.

Novel Chemical Process for Producing Chrome Coated Metal

PubMed Central

Pelar, Christopher; Greenaway, Karima; Zea, Hugo; Wu, Chun-Hsien

2018-01-01

This work demonstrates that a version of the Reduction Expansion Synthesis (RES) process, Cr-RES, can create a micron scale Cr coating on an iron wire. The process involves three steps. I. A paste consisting of a physical mix of urea, chrome nitrate or chrome oxide, and water is prepared. II. An iron wire is coated by dipping. III. The coated, and dried, wire is heated to ~800 °C for 10 min in a tube furnace under a slow flow of nitrogen gas. The processed wires were then polished and characterized, primarily with scanning electron microscopy (SEM). SEM indicates the chrome layer is uneven, but only on the scale of a fraction of a micron. The evidence of porosity is ambiguous. Elemental mapping using SEM electron microprobe that confirmed the process led to the formation of a chrome metal layer, with no evidence of alloy formation. Additionally, it was found that thickness of the final Cr layer correlated with the thickness of the precursor layer that was applied prior to the heating step. Potentially, this technique could replace electrolytic processing, a process that generates carcinogenic hexavalent chrome, but further study and development is needed. PMID:29303977

Novel Chemical Process for Producing Chrome Coated Metal.

PubMed

Pelar, Christopher; Greenaway, Karima; Zea, Hugo; Wu, Chun-Hsien; Luhrs, Claudia C; Phillips, Jonathan

2018-01-05

This work demonstrates that a version of the Reduction Expansion Synthesis (RES) process, Cr-RES, can create a micron scale Cr coating on an iron wire. The process involves three steps. I. A paste consisting of a physical mix of urea, chrome nitrate or chrome oxide, and water is prepared. II. An iron wire is coated by dipping. III. The coated, and dried, wire is heated to ~800 °C for 10 min in a tube furnace under a slow flow of nitrogen gas. The processed wires were then polished and characterized, primarily with scanning electron microscopy (SEM). SEM indicates the chrome layer is uneven, but only on the scale of a fraction of a micron. The evidence of porosity is ambiguous. Elemental mapping using SEM electron microprobe that confirmed the process led to the formation of a chrome metal layer, with no evidence of alloy formation. Additionally, it was found that thickness of the final Cr layer correlated with the thickness of the precursor layer that was applied prior to the heating step. Potentially, this technique could replace electrolytic processing, a process that generates carcinogenic hexavalent chrome, but further study and development is needed.

A mineralogical study in contrasts: highly mineralized whale rostrum and human enamel

NASA Astrophysics Data System (ADS)

Li, Zhen; Ai-Jawad, Maisoon; Siddiqui, Samera; Pasteris, Jill D.

2015-11-01

The outermost enamel of the human tooth and the rostrum of the whale Mesoplodon densirostris are two highly mineralized tissues that contain over 95 wt.% mineral, i.e., bioapatite. However, the same mineral type (carbonated hydroxylapatite) does not yield the same material properties, as revealed by Raman spectroscopy, scanning electron microscopy, electron microprobe analysis, and synchrotron X-ray diffraction analysis. Overall, the outermost enamel of a tooth has more homogeneous physical and chemical features than the rostrum. Chemical comparison of rostrum and enamel shows bioapatite in the rostrum to be enriched in Na, Mg, CO3, and S, whereas the outermost enamel shows only a slightly enriched Cl concentration. Morphologically, mineral rods (at tens of μm scale), crystallites and prisms (at μm and sub-μm scale), and platelets (at tens of nm scale) all demonstrate less organized texture in the rostrum than in enamel. Such contrasts between two mineralized tissues suggest distinct pathways of biomineralization, e.g., the nature of the equilibrium between mineral and body fluid. This study illustrates the remarkable flexibility of the apatite mineral structure to match its chemical and physical properties to specific biological needs within the same animal or between species.

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.

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.

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.

Adaption of synchronously scanned luminescence spectroscopy to organic-rich fluid inclusion microanalysis

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

Musgrave, J.A.; Carey, R.G.; Janecky, D.R.

1994-06-01

The instrumentation, the luminescence microprobe, and synchronously scanned luminescence spectroscopy technique described here can be used to classify microliter quantities of oil such as those in fluid inclusions in cements from petroleum reservoirs. It is primarily constructed to obtain synchronously scanned luminescence spectra from microscopic sized samples to characterize the organic classes of compounds that predominate. At present no other technique can so readily analyze a single oil-bearing fluid inclusion. The data collected from the technique are pertinent to evaluating systems and providing quantitative data for solving problems in oil migration and maturation determinations, oil-to-oil and oil-to-source correlations, oil degradation,more » and episodes and chemistry of cementation.« less

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.

Evidence for Rhythmicity Pacemaker in the Calcification Process of Scleractinian Coral

NASA Astrophysics Data System (ADS)

Gutner-Hoch, Eldad; Schneider, Kenneth; Stolarski, Jaroslaw; Domart-Coulon, Isabelle; Yam, Ruth; Meibom, Anders; Shemesh, Aldo; Levy, Oren

2016-02-01

Reef-building scleractinian (stony) corals are among the most efficient bio-mineralizing organisms in nature. The calcification rate of scleractinian corals oscillates under ambient light conditions, with a cyclic, diurnal pattern. A fundamental question is whether this cyclic pattern is controlled by exogenous signals or by an endogenous ‘biological-clock’ mechanism, or both. To address this problem, we have studied calcification patterns of the Red Sea scleractinian coral Acropora eurystoma with frequent measurements of total alkalinity (AT) under different light conditions. Additionally, skeletal extension and ultra-structure of newly deposited calcium carbonate were elucidated with 86Sr isotope labeling analysis, combined with NanoSIMS ion microprobe and scanning electron microscope imaging. Our results show that the calcification process persists with its cyclic pattern under constant light conditions while dissolution takes place within one day of constant dark conditions, indicating that an intrinsic, light-entrained mechanism may be involved in controlling the calcification process in photosymbiotic corals.

Characterization of boron carbide with an electron microprobe

NASA Technical Reports Server (NTRS)

Matteudi, G.; Ruste, J.

1983-01-01

Within the framework of a study of heterogeneous materials (Matteudi et al., 1971: Matteudi and Verchery, 1972) thin deposits of boron carbide were characterized. Experiments using an electronic probe microanalyzer to analyze solid boron carbide or boron carbide in the form of thick deposits are described. Quantitative results on boron and carbon are very close to those obtained when applying the Monte Carlo-type correction calculations.

Matrix vapor deposition/recrystallization and dedicated spray preparation for high-resolution scanning microprobe matrix-assisted laser desorption/ionization imaging mass spectrometry (SMALDI-MS) of tissue and single cells.

PubMed

Bouschen, Werner; Schulz, Oliver; Eikel, Daniel; Spengler, Bernhard

2010-02-01

Matrix preparation techniques such as air spraying or vapor deposition were investigated with respect to lateral migration, integration of analyte into matrix crystals and achievable lateral resolution for the purpose of high-resolution biological imaging. The accessible mass range was found to be beyond 5000 u with sufficient analytical sensitivity. Gas-assisted spraying methods (using oxygen-free gases) provide a good compromise between crystal integration of analyte and analyte migration within the sample. Controlling preparational parameters with this method, however, is difficult. Separation of the preparation procedure into two steps, instead, leads to an improved control of migration and incorporation. The first step is a dry vapor deposition of matrix onto the investigated sample. In a second step, incorporation of analyte into the matrix crystal is enhanced by a controlled recrystallization of matrix in a saturated water atmosphere. With this latter method an effective analytical resolution of 2 microm in the x and y direction was achieved for scanning microprobe matrix-assisted laser desorption/ionization imaging mass spectrometry (SMALDI-MS). Cultured A-498 cells of human renal carcinoma were successfully investigated by high-resolution MALDI imaging using the new preparation techniques. Copyright 2010 John Wiley & Sons, Ltd.

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.

Microprobe monazite geochronology: new techniques for dating deformation and metamorphism

NASA Astrophysics Data System (ADS)

Williams, M.; Jercinovic, M.; Goncalves, P.; Mahan, K.

2003-04-01

High-resolution compositional mapping, age mapping, and precise dating of monazite on the electron microprobe are powerful additions to microstructural and petrologic analysis and important tools for tectonic studies. The in-situ nature and high spatial resolution of the technique offer an entirely new level of structurally and texturally specific geochronologic data that can be used to put absolute time constraints on P-T-D paths, constrain the rates of sedimentary, metamorphic, and deformational processes, and provide new links between metamorphism and deformation. New analytical techniques (including background modeling, sample preparation, and interference analysis) have significantly improved the precision and accuracy of the technique and new mapping and image analysis techniques have increased the efficiency and strengthened the correlation with fabrics and textures. Microprobe geochronology is particularly applicable to three persistent microstructural-microtextural problem areas: (1) constraining the chronology of metamorphic assemblages; (2) constraining the timing of deformational fabrics; and (3) interpreting other geochronological results. In addition, authigenic monazite can be used to date sedimentary basins, and detrital monazite can fingerprint sedimentary source areas, both critical for tectonic analysis. Although some monazite generations can be directly tied to metamorphism or deformation, at present, the most common constraints rely on monazite inclusion relations in porphyroblasts that, in turn, can be tied to the deformation and/or metamorphic history. Examples will be presented from deep-crustal rocks of northern Saskatchewan and from mid-crustal rocks from the southwestern USA. Microprobe monazite geochronology has been used in both regions to deconvolute overprinting deformation and metamorphic events and to clarify the interpretation of other geochronologic data. Microprobe mapping and dating are powerful companions to mass spectroscopic dating techniques. They allow geochronology to be incorporated into the microstructural analytical process, resulting in a new level of integration of time (t) into P-T-D histories.

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.

As-Received, Ozone Cleaned and Ar+ Sputtered Surfaces of Hafnium Oxide Grown by Atomic Layer Deposition and Studied by XPS

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

Engelhard, Mark H.; Herman, Jacob A.; Wallace, Robert

2012-06-27

In this study, X-ray photoelectron spectroscopy (XPS) characterization was performed on 47 nm thick hafnium oxide (HfO{sub 2}) films grown by atomic layer deposition using TEMA-Hf/H{sub 2}O at 250 C substrate temperature. HfO{sub 2} is currently being studied as a possible replacement for Silicon Oxide (SiO{sub 2}) as a gate dielectric in electronics transistors. XPS spectra were collected on a Physical Electronics Quantum 2000 Scanning ESCA Microprobe using a monochromatic Al K{sub a} X-ray (1486.7 eV) excitation source. The sample was analyzed under the following conditions: as received, after UV irradiation for five minutes, and after sputter cleaning with 2more » kV Ar{sup +} ions for 180 seconds. Survey scans showed carbon, oxygen, and hafnium as the major species in the film, while the only minor species of argon and carbide was detected after sputtering. Adventitious carbon initially composed approximately 18.6 AT% of the surface, but after UV cleaning it was reduced to 2.4 AT%. This demonstrated that that the majority of carbon was due to adventitious carbon. However, after 2 kV Ar{sup +} sputtering there was still only trace amounts of carbon at {approx}1 AT%, Some of this trace carbon is now in the form of a carbide due to the interaction with Ar{sup +} used for sputter cleaning. Furthermore, the stoiciometric ratio of oxygen and hafnium is consistent with a high quality HfO{sub 2} film.« less

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.

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.

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.

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.

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

Microscopic and Metallurgical Aspects of the Space Shuttle Columbia Accident Investigation and Reconstruction

NASA Technical Reports Server (NTRS)

McDaniels, Steven J.

2004-01-01

The Space Shuttle Columbia was descending for a landing at the Kennedy Space Center (KSC) on February 1, 2003. Approximately 20 minutes prior to touchdown, the Columbia began disintegrating over the western United States; the majority of debris eventually impacted in eastern Texas and western Louisiana. A monumental effort eventually recovered approximately 84,000 pieces of debris, approximately 38% of the Orbiter's original dry weight. The debris was transported to KSC, where the items were catalogued and evaluated. Critical areas of interest, such as the left and right leading edge surfaces and the underside of the ship, were placed upon a grid to aid in the reconstruction. Items of interest included metallic structures, reinforced carbon-carbon composites, and ceramic heat insulation tiles. Many of the leading edge elements had re-solidified metallic deposits spattered on them. These deposits became known as slag and were one of the main focuses of the investigation. In order to help determine the sequence of events inside the left wing during the accident, the slag's composition, layering order, and directionality of deposition were studied. A myriad of analytical tests were performed in an attempt to ascertain the compositional and depositional characteristics of selected slag deposits, including the ordering of deposited layers within each individual slag deposit harvested. Initially, Scanning Electron Microscopy and Energy Dispersive X-Ray Spectroscopy (SEM/EDX) were performed to quickly characterize the overall composition of individual slag deposits: SEM utilizes a narrowlyfocused high-energy electron beam impinging upon a specimen. The incident beam excites and liberates lower energy secondary electrons, which are detected and analyzed, providing a visual representation of the sample's surface topography. EDX also relies on an incident electron beam, except an EDX unit measures X-ray energies generated by the impinging beam. Each element generates a unique X-ray signature; the EDX detector measures these discreet energies. EDX actually penetrates approximately 2 microns into the bulk of the sample. However, random examination of various portions of slag, coupled with the semiquantitative nature of the SEM/EDX analysis, did not yield convincingly pertinent data. Therefore, X-ray dot mapping was conducted, which provided more understandable data, both in terms of slag layering and composition. An X-ray dot map is generated by performing numerous EDX scans for individual elements, then compiling the scans in a visual representation. Eventually, specimens consisting of not only the slag, but of the adjacent RCC substrate as well were cross-sectioned. X-Ray dot mapping of the materialographicallymounted and -polished cross- sections provided a visual representation of both the layering sequence and compositional characteristics of the slag. Contemporaneously, Electron Spectroscopy for Chemical Analysis/X-Ray Photoelectron Spectroscopy (ESCA/XPS) and powdered X-Ray Diffraction (XRD) were performed to further characterize the deposits and to attempt to identify what, if any, compounds were present. The ESCA/XPS analysis allowed the analyst to "sputter" into the sample with an electron gun, aiding in the identification of the layering sequence. XPS uses photons, rather than electrons, which impinge upon the surface of the sample. XPS measures the electrons emitted from within the first 5 nm of the sample's surface. The XRD measures the scatter angles of incident X-rays; the angle and intensity of scatter depend upon the crystalline structure of the pulverized sample. XRD is considered a qualitative rather than quantitative technique. ESCA/XPS revealed that the final layer to deposit was predominantly carbonaceous. XRD was successful in identifying specific compounds, such as Al 2O3, Al and/or Al3 21SiO47, mullite (3(Al2)O3 -SiO2), and nickel-aluminides. Eventually, Electron MicroProbe Analysis (EMPA) was conducted on the marialographically-prepared cross- sections of selected slag deposits. Microprobe combines SEM and Wavelength Dispersive X-Ray Spectroscopy (WDS), and, like EDX, uses a narrowly-focused high-energy electron beam impinging upon a specimen to elicit, in the case of EPMA, characteristic X-rays with specific wavelengths. This quantitative, analytical tool proved the most useful in determining depositional layering and composition of the slag deposits. This information was utilized in verifying the location of the breach in the left leading edge of the wing of the Columbia.

Liquid oxygen LOX compatibility evaluations of aluminum lithium (Al-Li) alloys: Investigation of the Alcoa 2090 and MMC weldalite 049 alloys

NASA Technical Reports Server (NTRS)

Diwan, Ravinder M.

1989-01-01

The behavior of liquid oxygen (LOX) compatibility of aluminum lithium (Al-Li) alloys is investigated. Alloy systems of Alcoa 2090, vintages 1 to 3, and of Martin Marietta Corporation (MMC) Weldalite 049 were evaluated for their behavior related to the LOX compatibility employing liquid oxygen impact test conditions under ambient pressures and up to 1000 psi. The developments of these aluminum lithium alloys are of critical and significant interest because of their lower densities and higher specific strengths and improved mechanical properties at cryogenic temperatures. Of the different LOX impact tests carried out at the Marshall Space Flight Center (MSFC), it is seen that in certain test conditions at higher pressures, not all Al-Li alloys are LOX compatible. In case of any reactivity, it appears that lithium makes the material more sensitive at grain boundaries due to microstructural inhomogeneities and associated precipitate free zones (PFZ). The objectives were to identify and rationalize the microstructural mechanisms that could be relaxed to LOX compatibility behavior of the alloy system in consideration. The LOX compatibility behavior of Al-Li 2090 and Weldalite 049 is analyzed in detail using microstructural characterization techniques with light optical metallography, scanning electron microscopy (SEM), electron microprobe analysis, and surface studies using secondary ion mass spectrometry (SIMS), electron spectroscopy in chemical analysis (ESCA) and Auger electron spectroscopy (AES). Differences in the behavior of these aluminum lithium alloys are assessed and related to their chemistry, heat treatment conditions, and microstructural effects.

Alternatives for joining Si wafers to strain-accommodating Cu for high-power electronics

NASA Astrophysics Data System (ADS)

Faust, Nicholas; Messler, Robert W.; Khatri, Subhash

2001-10-01

Differences in the coefficients of thermal expansion (CTE) between silicon wafers and underlying copper electrodes have led to the use of purely mechanical dry pressure contacts for primary electrical and thermal connections in high-power solid-state electronic devices. These contacts are limited by their ability to dissipate I2R heat from within the device and by their thermal fatigue life. To increase heat dissipation and effectively deal with the CTE mismatch, metallurgical bonding of the silicon to a specially-structured, strain-accommodating copper electrode has been proposed. This study was intended to seek alternative methods for and demonstrate the feasibility of bonding Si to structured Cu in high-power solid-state devices. Three different but fundamentally related fluxless approaches identified and preliminarily assessed were: (1) conventional Sn-Ag eutectic solder; (2) a new, commercially-available active solder based on the Sn-Ag eutectic; and (3) solid-liquid interdiffusion bonding using the Au-In system. Metallurgical joints were made with varying quality levels (according to nonde-structive ultrasonic C-scan mapping, SEM, and electron microprobe) using each approach. Mechanical shear testing resulted in cohesive failure within the Si or the filler alloys. The best approach, in which eutectic Sn-Ag solder in pre-alloyed foil form was employed on Si and Cu substrates metallized (from the substrate outward) with Ti, Ni and Au, exhibited joint thermal conduction 74% better than dry pressure contacts.

[Interface bond and compatibility between Mark II machining ceramic and vita VM9 veneering porcelain].

PubMed

Liu, Tian-Shuang; Li, Zhen-Chun; Chen, Xiao-Dong

2009-04-01

To investigate the interface bond and thermal compatibility between Mark II machining ceramic and Vita VM9 veneering porcelain. A bar shaped specimen (30 mm x 15 mm x 1 mm in size) of Mark II block was prepared, with 0.5 mm-deep notch (vertical to the long axis of specimen) at the middle of the bottom surface. The upper surface was veneered with 0.3 mm VM9 dentin base porcelain. Then the specimen was fractured from the notching site and the fracture surface was examined under scanning electron microscope (SEM) and electron microprobe analyzer (EMPA) with electron beam of 1 microm in diameter. Another ten specimens (30 mm x 15 mm x 1.5 mm in size) were fabricated and the temperature of thermal shock resistance were tested. SEM observation showed tight bond between these two materials and EMPA results showed penetration of Al element from Mark II block into veneering porcelain and Ca element from veneering porcelain into Mark II block occurred after sintering baking. The average temperature of thermal shock resistance for specimens in this study was (194.0+/-10.3) degrees C. Cracks were mainly distributed in veneering porcelain. Chemical bond exists between the Mark II machining ceramic and Vita VM9 veneering porcelain, and there is good thermal compatibility between them.

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.

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

Electron-probe microanalysis of light elements in coal and other kerogen

USGS Publications Warehouse

Bustin, R.M.; Mastalerz, Maria; Raudsepp, M.

1996-01-01

Recent advances in electron microprobe technology including development of layered synthetic microstructures, more stable electronics and better matrix-correction programs facilitated routine microanalysis of the light elements in coal. Utilizing an appropriately equipped electron microprobe with suitable standards, it is now possible to analyze directly the light elements (C, O and N, if abundant) in coal macerals and other kerogen. The analytical results are both accurate compared to ASTM methods and highly precise, and provide an opportunity to access the variation in coal chemistry at the micrometre scale. Our experiments show that analyses using a 10 kV accelerating voltage and 10 nA beam current yield the most reliable data and result in minimum sample damage and contamination. High sample counts were obtained for C, O and N using a bi-elemental nickel-carbon pseudo-crystal (2d = 9.5 nm) as an analyzing crystal. Vitrinite isolated from anthracite rank coal proves the best carbon standard and is more desirable than graphite which has higher porosity, whereas lower rank vitrinite is too heterogeneous to use routinely as a standard. Other standards utilized were magnesite for oxygen and BN for nitrogen. No significant carbon, oxygen or nitrogen X-ray peak shifts or peak-shape changes occur between standards and the kerogen analyzed. Counting rates for carbon and oxygen were found to be constant over a range of beam sizes and currents for counting times up to 160 s. Probe-determined carbon and oxygen contents agree closely with those reported from ASTM analyses. Nitrogen analyses compare poorly to ASTM values which probably is in response to overlap between the nitrogen Ka peak with the carbon K-adsorption edge and the overall low nitrogen content of most of our samples. Our results show that the electron microprobe technique provides accurate compositional data for both minor and major elements in coal without the necessity and inherent problems associated with mechanically isolating macerals. Studies to date have demonstrated the level of compositional variability within and between macerals in suites of Canadian coals.

Impact of quaternary climate on seepage at Yucca Mountain, Nevada

USGS Publications Warehouse

Whelan, J.F.; Paces, J.B.; Neymark, L.A.; Schmitt, A.K.; Grove, M.

2006-01-01

Uranium-series ages, oxygen-isotopic compositions, and uranium contents were determined in outer growth layers of opal and calcitefrom 0.5- to 3-centimeter-thick mineral coatings hosted by lithophysal cavities in the unsaturated zone at Yucca Mountain, Nevada, the proposed site of a permanent repository for high-level radioactive waste. Micrometer-scale growth layering in the minerals was imaged using a cathodoluminescence detector on a scanning electron microscope. Determinations of the chemistry, ages, and delta oxygen-18 (??18O) values of the growth layers were conducted by electron microprobe analysis and secondary ion mass spectrometry techniques at spatial resolutions of 2 to about 20 micrometers (??m) and 25 to 40 ??m, respectively. Growth rates for the last 300 thousand years (k.y.) calculated from about 300 new high-resolution uranium-series ages range from approximately 0.5 to 1.5 ??m/k.y. for 1- to 3-centimeter-thick coatings, whereas coatings less than about 1-centimeter-thick have growth rates less than 0.5 ??m/k.y. At the depth of the proposed repository, correlations of uranium concentration and ??18O values with regional climate records indicate that unsaturated zone percolation and seepage water chemistries have responded to changes in climate during the last several hundred thousand years.

Vanadium Geochemistry of Oil Sands Fluid Petroleum Coke.

PubMed

Nesbitt, Jake A; Lindsay, Matthew B J

2017-03-07

Vanadium has previously been linked to elevated toxicity of leachates derived from oil sands petroleum coke. However, geochemical controls on V mobility within coke deposits remain poorly constrained. Detailed examinations of porewater and solid-phase V geochemistry were therefore performed on oil sands fluid petroleum coke deposits in Alberta, Canada. Sample collection focused on both active and reclaimed deposits, which contained more than 3 × 10 7 m 3 of fluid petroleum coke. Dissolved V concentrations were highest (up to 3.0 mg L -1 ) immediately below the water table but decreased rapidly with increasing depth. This trend corresponded to a transition from mildly acidic (pH 6-7) and oxic conditions to mildly alkaline (pH 7-8.5) and anoxic conditions. Scanning electron microscopy (SEM), electron microprobe analysis (EMPA), and micro-X-ray fluorescence (μXRF) mapping revealed coke particles exhibited an internal structure characterized by successive concentric layers. The outer margins of these layers were characterized by elevated V, Fe, Si, and Al concentrations, indicating the presence of inorganic phases. Micro-X-ray absorption near-edge structure (μXANES) spectroscopy revealed that V speciation was dominated by V(IV) porphyrins except at outer margins of layers, where octahedrally coordinated V(III) was a major component. Minor to trace V(V) was also detected within fluid petroleum coke particles.

Mode of occurrence of chromium in four US coals

USGS Publications Warehouse

Huggins, Frank E.; Shah, N.; Huffman, G.P.; Kolker, A.; Crowley, S.; Palmer, C.A.; Finkelman, R.B.

2000-01-01

The mode of occurrence of chromium in three US bituminous coals and one US subbituminous has been examined using both X-ray absorption fine structure (XAFS) spectroscopy and a selective leaching protocol supplemented by scanning electron microscopy (SEM) and electron microprobe measurements. A synthesis of results from both methods indicates that chromium occurs principally in two forms in the bituminous coals: the major occurrence of chromium is associated with the macerals and is not readily leached by any reagent, whereas a second, lesser occurrence, which is leachable in hydrofluoric acid (HF), is associated with the clay mineral, illite. The former occurrence is believed to be a small particle oxyhydroxide phase (CrO(OH)). One coal also contained a small fraction (<5%) of the chromium in the form of a chromian magnetite, and the leaching protocol indicated the possibility of a similar small fraction of chromium in sulfide form in all three coals. There was little agreement between the two techniques on the mode of occurrence of chromium in the subbituminous coal; however, only a limited number of subbituminous coals have been analyzed by either technique. The chromium in all four coals was trivalent as no evidence was found for the Cr6+ oxidation state in any coal.

Microstructure Evolution During Stainless Steel-Copper Vacuum Brazing with a Ag/Cu/Pd Filler Alloy: Effect of Nickel Plating

NASA Astrophysics Data System (ADS)

Choudhary, R. K.; Laik, A.; Mishra, P.

2017-03-01

Vacuum brazing of stainless steel and copper plates was done using a silver-based filler alloy. In one set of experiments, around 30-µm-thick nickel coatings were electrochemically applied on stainless steel plates before carrying out the brazing runs and its effect in making changes in the braze-zone microstructure was studied. For brazing temperature of 830 °C, scanning electron microscopy examination of the braze-zone revealed that relatively sound joints were obtained when brazing was done with nickel-coated stainless steel than with uncoated one. However, when brazing of nickel-coated stainless steel and copper plates was done at 860 °C, a wide crack appeared in the braze-zone adjacent to copper side. Energy-dispersive x-ray analysis and electron microprobe analysis confirmed that at higher temperature, the diffusion of Cu atoms from copper plate towards the braze-zone was faster than that of Ni atoms from nickel coating. Helium leak rate of the order 10-11 Pa m3/s was obtained for the crack-free joint, whereas this value was higher than 10-4 Pa m3/s for the joint having crack. The shear strength of the joint was found to decrease considerably due to the presence of crack.

Cellular distribution of uranium after acute exposure of renal epithelial cells: SEM, TEM and nuclear microscopy analysis

NASA Astrophysics Data System (ADS)

Carrière, Marie; Gouget, Barbara; Gallien, Jean-Paul; Avoscan, Laure; Gobin, Renée; Verbavatz, Jean-Marc; Khodja, Hicham

2005-04-01

The major health effect of uranium exposure has been reported to be chemical kidney toxicity, functional and histological damages being mainly observed in proximal tubule cells. Uranium enters the proximal tubule as uranyl-bicarbonate or uranyl-citrate complexes. The aim of our research is to investigate the mechanisms of uranium toxicity, intracellular accumulation and repartition after acute intoxication of rat renal proximal tubule epithelial cells, as a function of its chemical form. Microscopic observations of renal epithelial cells after acute exposure to uranyl-bicarbonate showing the presence of intracellular precipitates as thin needles of uranyl-phosphate localized in cell lysosomes have been published. However the initial site of precipitates formation has not been identified yet: they could either be formed outside the cells before internalization, or directly inside the cells. Uranium solubility as a function and initial concentration was specified by ICP-MS analysis of culture media. In parallel, uranium uptake and distribution in cell monolayers exposed to U-bicarbonate was investigated by nuclear microprobe analyses. Finally, the presence of uranium precipitates was tested out by scanning electron microscopic observations (SEM), while extracellular and/or intracellular precipitates were observed on thin sections of cells by transmission electron microscopy (TEM).

Long-term thermal degradation and alloying constituent effects on five boron/aluminum composites

NASA Technical Reports Server (NTRS)

Olsen, G. C.

1982-01-01

Thermal exposure effects on the properties of five boron/aluminum composite systems were experimentally investigated. The composite systems were 49 volume percent boron fibers (203 micron diameter) in aluminum-alloy matrices 1100 Al, 2024 Al, 3003 Al, 5052 Al, and 6061 Al. Specimens were thermally exposed up to 10,000 hours at 500 K and 590 K, up to 500 hours at 730 K, and up to 10,000 hours at 500 K and 590 K, up to 500 hours at 730 K, and up to 2000 thermal cycles between 200 K and 590 K. Composite longitudinal and transverse tensile strengths, longitudinal compression strength, and in-plane shear strength were determined. None of the systems was severely degraded by exposure at 590 K. The best performing system was B-2024 Al. Effects of matrix alloys on degradation mechanisms were experimentally investigated. Composite specimens and individual fibers were metallurgically analyzed with a scanning electron microscope and an electron microprobe to determine failure characteristics, chemical element distribution, and reaction layer morphology. Alloying constituents were found to be affect the composite degradation mechanisms as follows: alloys containing iron, but without manganese as a stabilizer, caused increased low-temperature degradation; alloys containing magnesium, iron, or manganese caused increased degradation; and alloys containing copper caused increased fiber strength.

Timescales of magmatic processes prior to the ˜4.7 ka Agnano-Monte Spina eruption (Campi Flegrei caldera, Southern Italy) based on diffusion chronometry from sanidine phenocrysts

NASA Astrophysics Data System (ADS)

Iovine, Raffaella Silvia; Fedele, Lorenzo; Mazzeo, Fabio Carmine; Arienzo, Ilenia; Cavallo, Andrea; Wörner, Gerhard; Orsi, Giovanni; Civetta, Lucia; D'Antonio, Massimo

2017-02-01

Barium diffusion chronometry applied to sanidine phenocrysts from the trachytic Agnano-Monte Spina eruption (˜4.7 ka) constrains the time between reactivation and eruption of magma batches in the Campi Flegrei caldera. Backscattered electron imaging and quantitative electron microprobe measurements on 50 sanidine phenocrysts from representative pumice samples document core-to-rim compositional zoning. We focus on compositional breaks near the crystal rims that record magma mixing processes just prior to eruption. Diffusion times were modeled at a magmatic temperature of 930 °C using profiles based on quantitative BaO point analyses, X-ray scans, and grayscale swath profiles, yielding times ≤60 years between mixing and eruption. Such short timescales are consistent with volcanological and geochronological data that indicate that at least six eruptions occurred in the Agnano-San Vito area during few centuries before the Agnano-Monte Spina eruption. Thus, the short diffusion timescales are similar to time intervals between eruptions. Therefore, the rejuvenation time of magma residing in a shallow reservoir after influx of a new magma batch that triggered the eruption, and thus pre-eruption warning times, may be as short as years to a few decades at Campi Flegrei caldera.

Reservoir heterogeneity in Carter Sandstone, North Blowhorn Creek oil unit and vicinity, Black Warrior Basin, Alabama

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

Kugler, R.L.; Pashin, J.C.

1992-05-01

This report presents accomplishments made in completing Task 3 of this project which involves development of criteria for recognizing reservoir heterogeneity in the Black Warrior basin. The report focuses on characterization of the Upper Mississippian Carter sandstone reservoir in North Blowhorn Creek and adjacent oil units in Lamar County, Alabama. This oil unit has produced more than 60 percent of total oil extracted from the Black Warrior basin of Alabama. The Carter sandstone in North Blowhorn Creek oil unit is typical of the most productive Carter oil reservoirs in the Black Warrior basin of Alabama. The first part of themore » report synthesizes data derived from geophysical well logs and cores from North Blowhorn Creek oil unit to develop a depositional model for the Carter sandstone reservoir. The second part of the report describes the detrital and diagenetic character of Carter sandstone utilizing data from petrographic and scanning electron microscopes and the electron microprobe. The third part synthesizes porosity and pore-throat-size-distribution data determined by high-pressure mercury porosimetry and commercial core analyses with results of the sedimentologic and petrographic studies. The final section of the report discusses reservoir heterogeneity within the context of the five-fold classification of Moore and Kugler (1990).« less

Seaching for a Silver Lining: Using Pb Isotopes to Constrain the Source of Argentiferous Galena at La Isabela

NASA Astrophysics Data System (ADS)

Thibodeau, A. M.; Killick, D. J.; Ruiz, J.; Chesley, J. T.; Baker, M.

2005-12-01

This study investigates the smelting and refining of argentiferous galena at La Isabela, Dominican Republic (1493-1498), the town founded by Columbus on his second voyage to the Americas. Archaeologists recovered approximately 100 kilograms of galena and 200 kilograms of metallurgical slag near the remains of a crude furnace unearthed at the site (Deagan and Cruxent 2002). The purpose of this study was to determine if these remains are evidence that members of Columbus's fleet prospected for silver during his second expedition. Samples of ore and slag were examined as metallographic polished sections, and petrographic thin sections by optical and scanning electron microscopes. The composition of the ore and slag allows us to infer these ores were processed in a two-stage procedure to produce silver metal and a lead silicate slag. Electron microprobe analysis of galena indicates highly variable but low Ag content (50 ppm), which may account for the fact some of the ore was left unprocessed. Lead isotope analysis by multi-collector ICP-MS indicates that the galena likely came from a single source and was not mined within the Caribbean. Instead, the isotopic signature of these ores is consistent with an Old World source, possibly in the Linares-La Carolina Pb-Zn vein field of southwestern Spain.

Isomorphism and solid solutions among Ag- and Au-selenides

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

Palyanova, Galina A.; Seryotkin, Yurii V.; Novosibirsk State University

Au-Ag selenides were synthesized by heating stoichiometric mixtures of elementary substances of initial compositions Ag{sub 2−x}Au{sub x}Se with a step of x=0.25 (0≤x≤2) to 1050 °C and annealing at 500 °C. Scanning electron microscopy, optical microscopy, electron microprobe analysis and X-ray powder diffraction methods have been applied to study synthesized samples. Results of studies of synthesized products revealed the existence of three solid solutions with limited isomorphism Ag↔Au: naumannite Ag{sub 2}Se – Ag{sub 1.94}Au{sub 0.06}Se, fischesserite Ag{sub 3}AuSe{sub 2} - Ag{sub 3.2}Au{sub 0.8}Se{sub 2} and gold selenide AuSe - Au{sub 0.94}Ag{sub 0.06}Se. Solid solutions and AgAuSe phases were added tomore » the phase diagram of Ag-Au-Se system. Crystal-chemical interpretation of Ag-Au isomorphism in selenides was made on the basis of structural features of fischesserite, naumannite, and AuSe. - Highlights: • Au-Ag selenides were synthesized. • Limited Ag-Au isomorphism in the selenides is affected by structural features. • Some new phases were introduced to the phase diagram Ag-Au-Se.« less

Analysis of Phase Separation in Czochralski Grown Single Crystal Ilmenite

NASA Technical Reports Server (NTRS)

Wilkins, R.; Powell, Kirk St. A.; Loregnard, Kieron R.; Lin, Sy-Chyi; Muthusami, Jayakumar; Zhou, Feng; Pandey, R. K.; Brown, Geoff; Hawley, M. E.

1998-01-01

Ilmenite (FeTiOs) is a wide bandgap semiconductor with an energy gap of 2.58 eV. Ilmenite has properties suited for radiation tolerant applications, as well as a variety of other electronic applications. Single crystal ilmenite has been grown from the melt using the Czochralski method. Growth conditions have a profound effect on the microstructure of the samples. Here we present data from a variety of analytical techniques which indicate that some grown crystals exhibit distinct phase separation during growth. This phase separation is apparent for both post-growth annealed and unannealed samples. Under optical microscopy, there appear two distinct areas forming a matrix with an array of dots on order of 5 pm diameter. While appearing bright in the optical micrograph, atomic force microscope (AFM) shows the dots to be shallow pits on the surface. Magnetic force microscope (MFM) shows the dots to be magnetic. Phase identification via electron microprobe analysis (EMPA) indicates two major phases in the unannealed samples and four in the annealed samples, where the dots appear to be almost pure iron. This is consistent with micrographs taken with a scanning probe microscope used in the magnetic force mode. Samples that do not exhibit the phase separation have little or no discernible magnetic structure detectable by the MFM.

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

Ouyang, J.H.; Li, X.; Lei, T.C.

The microstructure of a laser-clad TiC-Ni particle-reinforced coating on 1045 steel was studied by scanning electron microscopy (SEM), transmission electron microscopy (TEM), and ion microprobe mass spectroscopy (IMMS). The microstructural constituents of the clad layers (CLs) were analyzed to be TiC particles, {gamma}-Ni primary dendrites, and interdendritic eutectics of {gamma}{sub E}-Ni plus M{sub 23}(CB){sub 6} and M{sub 6}(CB) carboborides. Three growth mechanisms of the original TiC particles were found: (1) stepped lateral growth at the edges, (2) radiated and cylindrically coupled growth at the edges, and (3) bridging growth of the clustered particles. Ordered and modulated structures were found inmore » the original TiC particles. In addition to the original TiC particles, fine TiC particles precipitated from the liquid phase and {gamma}-Ni solid solution during laser cladding. The microstructures of the bonding zones (BZs) were intimately associated with laser processing parameters. The BZs of the clad coatings can be categorized into three types according to the combination of the CL with heat-affected zone (HAZ): (1) straight interface combination, (2) zigzag connection, and (3) combination by partial melting of prior austenitic grain boundaries of the substrate. The microstructural evolution of the CLs was discussed. The formation and phase transformation models of the BZs were proposed.« less

Bone growth and bone development in the presence of implants or after induced leg-lengthening studied using the Oxford Scanning Proton Microprobe

NASA Astrophysics Data System (ADS)

Pålsgård, Eva; Johansson, Carina; Li, Gang; Grime, Geoff W.; Triffitt, J. T.

1997-07-01

To respond to varying environmental demands the bone tissue in the body is under continual reconstruction throughout life. It is known that metallic elements are important for maintaining normal bone structure, but their roles are not well understood. More information about the effects of metal excess or deficiency is needed to help in the development of metallic bone implants and to improve the treatment of bone fractures and defects. The Oxford Scanning Proton Microprobe (SPM) is being applied in two studies involving metal ions in bone: (1) bone regrowth and bonding to titanium bone implants may be influenced by diffusion of Ti ions into the bone. We are using microPIXE to determine the metal ion content of bone developing in contact with implants of pure Nb, Ti and Ti alloys. (2) Bone lengthening as a surgical procedure is induced by fracturing the bone and allowing it to heal with a small gap between the fractured ends created by the use of external fixators. The gap can be slowly increased during the healing process to stimulate the production of new bone. The enzymes and other constituents of the developing bone need certain metals for their function. Using experimental animals we have studied the concentrations of the metals and whether a deficiency of trace metals limits the optimum rate of bone lengthening.

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.

Structural and compositional characterization of synthetic (Ca,Sr)-tremolite and (Ca,Sr)-diopside solid solutions

NASA Astrophysics Data System (ADS)

Gottschalk, M.; Najorka, J.; Andrut, M.

Tremolite (CaxSr1-x)2Mg5[Si8O22/(OH)2] and diopside (CaxSr1-x)Mg[Si2O6] solid solutions have been synthesized hydrothermally in equilibrium with a 1 molar (Ca,Sr)Cl2 aqueous solution at 750°C and 200 MPa. The solid run products have been investigated by optical, electron scanning and high resolution transmission electron microscopy, electron microprobe, X-ray-powder diffraction and Fourier-transform infrared spectroscopy. The synthesized (Ca,Sr)-tremolites are up to 2000 µm long and 30 µm wide, the (Ca,Sr)-diopsides are up to 150 µm long and 20 µm wide. In most runs the tremolites and diopsides are well ordered and chain multiplicity faults are rare. Nearly pure Sr-tremolite (tr0.02Sr-tr0.98) and Sr-diopside (di0.01Sr-di0.99) have been synthesized. A continuous solid solution series, i.e. complete substitution of Sr2+ for Ca2+ on M4-sites exists for (Ca,Sr)-tremolite. Total substitution of Sr2+ for Ca2+ on M2-sites can be assumed for (Ca,Sr)-diopsides. For (Ca,Sr)-tremolites the lattice parameters a, b and β are linear functions of composition and increase with Sr-content whereas c is constant. For the diopside series all 4 lattice parameters are a linear function of composition; a, b, c increase and β decreases with rising Sr-content. The unit cell volume for tremolite increases 3.47% from 906.68 Å3 for tremolite to 938.21 Å3 for Sr-tremolite. For diopside the unit cell volume increases 4.87 % from 439.91 Å3 for diopside to 461.30 Å3 for Sr-diopside. The observed splitting of the OH stretching band in tremolite is caused by different configurations of the next nearest neighbors (multi mode behavior). Resolved single bands can be attributed to the following configurations on the M4-sites: SrSr, SrCa, CaCa and CaMg. The peak positions of these 4 absorption bands are a linear function of composition. They are shifted to lower wavenumbers with increasing Sr-content. No absorption band due to the SrMg configuration on the M4-site is observed. This indicates a very low or negligible cummingtonite component in Sr-rich tremolites, which is also supported by electron microprobe analysis.

Possibilities of LA-ICP-MS technique for the spatial elemental analysis of the recent fish scales: Line scan vs. depth profiling

NASA Astrophysics Data System (ADS)

Holá, Markéta; Kalvoda, Jiří; Nováková, Hana; Škoda, Radek; Kanický, Viktor

2011-01-01

LA-ICP-MS and solution based ICP-MS in combination with electron microprobe are presented as a method for the determination of the elemental spatial distribution in fish scales which represent an example of a heterogeneous layered bone structure. Two different LA-ICP-MS techniques were tested on recent common carp ( Cyprinus carpio) scales: A line scan through the whole fish scale perpendicular to the growth rings. The ablation crater of 55 μm width and 50 μm depth allowed analysis of the elemental distribution in the external layer. Suitable ablation conditions providing a deeper ablation crater gave average values from the external HAP layer and the collagen basal plate. Depth profiling using spot analysis was tested in fish scales for the first time. Spot analysis allows information to be obtained about the depth profile of the elements at the selected position on the sample. The combination of all mentioned laser ablation techniques provides complete information about the elemental distribution in the fish scale samples. The results were compared with the solution based ICP-MS and EMP analyses. The fact that the results of depth profiling are in a good agreement both with EMP and PIXE results and, with the assumed ways of incorporation of the studied elements in the HAP structure, suggests a very good potential for this method.

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

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.

Mechanical, Chemical and Microstructural Characterization of Monazite-Coated Silicon Carbide Fibers

NASA Technical Reports Server (NTRS)

Bansal, N. P.; Wheeler, D. R.; Chen, Y. L.

2000-01-01

Tensile strengths of as-received Hi-Nicalon and Sylramic fibers and those having monazite surface coatings, deposited by atmospheric pressure chemical vapor deposition, were measured at room temperature and the Weibull statistical parameters determined. The average tensile strengths of uncoated Hi-Nicalon and Sylramic fibers were 3.19 +/- 0.73 and 2.78 +/- 0.53 GPa with a Weibull modulus of 5.41 and 5.52, respectively. The monazite-coated Hi-Nicalon and Sylramic fibers showed strength loss of approx. 10 and 15 percent, respectively, compared with the as-received fibers. The elemental compositions of the fibers and the coatings were analyzed using scanning Auger microprobe and energy dispersive X-ray spectroscopy. The LaPO4 coating on Hi-Nicalon fibers was approximately stoichiometric and about 50 nm thick. The coating on the Sylramic fibers extended to a depth of about 100 to 150 nm. The coating may have been stoichiometric LaPO4 in the first 30 to 40 nm of the layer. However, the surface roughness of Sylramic fiber made this profile somewhat difficult to interpret. Microstructural analyses of the fibers and the coatings were done by scanning electron microscopy, transmission electron microscopy, and selected area electron diffraction. Hi-Nicalon fiber consists of fine beta-SiC nanocrystals ranging in size from 1 to 30 mn embedded in an amorphous matrix. Sylramic is a polycrystalline stoichiometric silicon carbide fiber consisting of submicron beta-SiC crystallites ranging from 100 to 300 nm. Small amount of TiB2 nanocrystallites (approx. 50 nm) are also present. The LaPO4 coating on Hi-Nicalon fibers consisted of a chain of peanut shape particles having monazite-(La) structure. The coating on Sylramic fibers consisted of two layers. The inner layer was a chain of peanut shape particles having monazite-(La) structure. The outer layer was comprised of much smaller particles with a microcrystalline structure.

Microstructural, Chemical and Mechanical Characterization of Polymer-Derived Hi-Nicalon Fibers with Surface Coatings

NASA Technical Reports Server (NTRS)

Bansal, Narottam P.; Chen, Yuan L.

1998-01-01

Room temperature tensile strengths of as-received Hi-Nicalon fibers and those having BN/SiC, p-BN/SiC, and p-B(Si)N/SiC surface coatings, deposited by chemical vapor deposition, were measured using an average fiber diameter of 13.5 microns. The Weibull statistical parameters were determined for each fiber. The average tensile strength of uncoated Hi-Nicalon on was 3.19 +/- 0.73 GPa with a Weibull modulus of 5.41. Strength of fibers coated with BN/SiC did not change. However, coat with p-BN/SiC and p-B(Si)N/SiC surface layers showed strength loss of approx. 10 and 35 percent, respectively, compared with as-received fibers. The elemental compositions of the fibers and the coatings were analyzed using scanning Auger microprobe and energy dispersive x-ray spectroscopy. The BN coating was contaminated with a large concentration of carbon and some oxygen. In contrast, p-BN, p-B(Si)N, and SiC coatings did not show any contamination. Microstructural analyses of the fibers and the coatings were done by scanning electron microscopy (SEM), transmission electron microscopy (TEM), and selected area electron diffraction. Hi-Nicalon fiber consists of the P-SIC nanocrystals ranging in size from 1 to 30 nm embedded in an amorphous matrix. TEM analysis of the BN coating revealed four distinct layers with turbostatic structure. The p-BN layer was turbostratic and showed considerable preferred orientation. The p-B(Si)N was glassy and the silicon and boron were uniformly distributed. The silicon carbide coating was polycrystalline with a columnar structure along the growth direction. The p-B(Si)N/SiC coatings were more uniform, less defective and of better quality than the BN/SiC or the p-BN/SiC coatings.

The first investigative science-based evidence of Morgellons psychogenesis.

PubMed

Roncati, Luca; Gatti, Antonietta Morena; Pusiol, Teresa; Piscioli, Francesco; Barbolini, Giuseppe; Maiorana, Antonio

2016-01-01

Morgellons disease is an infrequent syndromic condition, that typically affects middle-aged white women, characterized by crawling sensations on and under the skin, associated with itchy rashes, stinging sores, fiber-like filaments emerging from the sores, severe fatigue, concentrating difficulty, and memory loss. The scientific community is prone to believe that Morgellons is the manifestation of various psychiatric syndromes (Munchausen, Munchausen by proxy, Ekbom, Wittmaack-Ekbom). Up until now, no investigative science-based evidence about its psychogenesis has ever been provided. In order to close this gap, we have analyzed the filaments extracted from the skin lesions of a 49-year-old Caucasian female patient, by using a Field Emission Gun-Environmental Electron Scanning Microscope equipped with an X-ray microprobe, for the chemico-elemental characterization of the filaments, comparing them with those collected during a detailed indoor investigation, with careful air monitoring, in her apartment. Our results prove the self-introduction under the epidermis of environmental filaments. For the first time in the literature, we have scientifically demonstrated the self-induced nature of Morgellons disease, thereby wiping out fanciful theories about its etiopathogenesis.

Coexistence of three calcium carbonate polymorphs in the shell of the Antarctic clam Laternula elliptica

NASA Astrophysics Data System (ADS)

Nehrke, Gernot; Poigner, Harald; Wilhelms-Dick, Dorothee; Brey, Thomas; Abele, Doris

2012-05-01

We analyzed shell cuts of five individuals of the Antarctic bivalve Laternula elliptica from three locations along the Antarctic Peninsula by means of Confocal Raman Microscopy (CRM) as well as Electron Microprobe (EMP). The shell of L. elliptica has been previously described as being composed of aragonite exclusively. Now, CRM mapping reveals that three polymorphs of calcium carbonate - aragonite, calcite, and vaterite - are present in the chondrophore region of the examined individuals. Annual shell growth layers continue through aragonite and vaterite, suggesting simultaneous mineralization of both polymorphs. Spatially congruent EMP scans showed that the calcium carbonate polymorph affects the distribution of magnesium and strontium within the chondrophore. This is, to our knowledge, the first report of the coexistence of these three calcium carbonate polymorphs within the mineralized structures of a marine calcifying organism. Particularly the presence of vaterite is unexpected, but shows striking similarities to some fish otoliths. The strong effect of the calcium carbonate polymorph on trace element incorporation restrict the suitability of magnesium and strontium based proxies for the chondrophore area of L. elliptica.

Macrosegregation of GeSi Alloys Grown in a Static Magnetic Field

NASA Technical Reports Server (NTRS)

Ritter, T. M.; Volz, M. P.; Cobb, S. D.; Szofran, F. R.

1999-01-01

Axial and radial macrosegregation profiles have been determined for GeSi alloy crystals grown by the vertical Bridgman technique. An axial 5 Tesla magnetic field was applied to several samples during growth to decrease the melt velocities by means of the Lorentz force. Compositions were measured with either energy dispersive X-ray spectroscopy (EDS) on a scanning electron microscope (SEM) or by wavelength dispersive X-ray spectroscopy (WDS) on a microprobe. The crystals were processed in graphite, hot-pressed boron nitride (BN), and pyrolytic boron nitride (PBN) ampoules, which produced various solid-liquid interface shapes during solidification. Those samples grown in a graphite ampoule exhibited radial profiles consistent with a highly concave interface and axial profiles indicative of complete mixing in the melt. The samples grown in BN and PBN ampoules had less radial variation. Axial macrosegregation profiles of these samples fell between the predictions for a completely mixed melt and one where solute transport is dominated by diffusion. Possible explanations for the apparent insufficiency of the magnetic field to achieve diffusion controlled growth conditions are discussed.

Post-flight analyses of the crystals from the M0003-14 quartz crystal microbalance experiment

NASA Technical Reports Server (NTRS)

Stuckey, W. K.; Radhakrishnan, G.; Wallace, D.

1993-01-01

Quartz Crystal Microbalances constructed by QCM Research were flown on the leading and trailing edges of LDEF as one of the sub-experiments of M0003. Response of the crystals coated with 150 A of In2O3 was recorded during the first 424 days of the mission. A second QCM with crystals coated with 150 A of ZnS was also flown but not monitored. After the flight, the QCM's were disassembled and analyzed in The Aerospace Corporation laboratories. The samples included the crystals from the leading and trailing edge samples of both types of coatings along with the reference crystals, which were inside the QCM housing. Analyses were performed by scanning electron microscopy, energy dispersive x-ray analyses, x-ray photoelectron spectroscopy, ion microprobe mass analysis, and reflectance spectroscopy in the infrared and UV/visible regions. The crystals are contaminated predominantly with silicone compounds. The contamination is higher on the leading edge than on the trailing edge and higher on the exposed crystals than on the reference crystals.

Oxidation of ZrB2 SiC TaSi2 Materials at Ultra High Temperatures

NASA Technical Reports Server (NTRS)

Opila, E.; Smith, J.; Levine, S.; Lorincz, J.; Reigel, M.

2008-01-01

ZrB2 - 20v% SiC - 20v% TaSi2 was oxidized in stagnant air for ten minute cycles for times up to 100 minutes at 1627 C and 1927 C. The sample oxidized at 1627 C showed oxidation resistance better than that of the standard ZrB2 - 20v% SiC. The sample oxidized at 1927 C, however, showed evidence of liquid phase formation and complex oxidation products. The sample exposed at 1927 C was analyzed in detail by scanning electron microprobe and wavelength dispersive spectroscopy to understand the complex oxidation and melting reactions occurring during exposure. The as hot-pressed material shows the formation of a Zr(Ta)B2 phase in addition to the three phases in the nominal composition already noted. After oxidation, the TaSi2 in the matrix was completely reacted to form Ta(Zr)C. The layered oxidation products included SiO2, ZrO2, Ta2O5, and a complex oxide containing both Zr and Ta. Likely reactions are proposed based on thermodynamic phase stability and phase morphology.

Characterization of the interface between the bulk glass forming alloy Zr{sub 41}Ti{sub 14}Cu{sub 12}Ni{sub 10}Be{sub 23} with pure metals and ceramics

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

Schroers, Jan; Samwer, Konrad; Szuecs, Frigyes

The reaction of the bulk glass forming alloy Zr{sub 41}Ti{sub 14}Cu{sub 12}Ni{sub 10}Be{sub 23} (Vit 1) with W, Ta, Mo, AlN, Al{sub 2}O{sub 3}, Si, graphite, and amorphous carbon was investigated. Vit 1 samples were melted and subsequently solidified after different processing times on discs of the different materials. Sessile drop examinations of the macroscopic wetting of Vit 1 on the discs as a function of temperature were carried out in situ with a digital optical camera. The reactions at the interfaces between the Vit 1 sample and the different disc materials were investigated with an electron microprobe. The structuremore » and thermal stability of the processed Vit 1 samples were examined by x-ray diffraction and differential scanning calorimetry. The results are discussed in terms of possible applications for composite materials. (c) 2000 Materials Research Society.« less

Joining Dental Ceramic Layers With Glass

PubMed Central

Saied, MA; Lloyd, IK; Haller, WK; Lawn, BR

2011-01-01

Objective Test the hypothesis that glass-bonding of free-form veneer and core ceramic layers can produce robust interfaces, chemically durable and aesthetic in appearance and, above all, resistant to delamination. Methods Layers of independently produced porcelains (NobelRondo™ Press porcelain, Nobel BioCare AB and Sagkura Interaction porcelain, Elephant Dental) and matching alumina or zirconia core ceramics (Procera alumina, Nobel BioCare AB, BioZyram yttria stabilized tetragonal zirconia polycrystal, Cyrtina Dental) were joined with designed glasses, tailored to match thermal expansion coefficients of the components and free of toxic elements. Scanning electron microprobe analysis was used to characterize the chemistry of the joined interfaces, specifically to confirm interdiffusion of ions. Vickers indentations were used to drive controlled corner cracks into the glass interlayers to evaluate the toughness of the interfaces. Results The glass-bonded interfaces were found to have robust integrity relative to interfaces fused without glass, or those fused with a resin-based adhesive. Significance The structural integrity of the interfaces between porcelain veneers and alumina or zirconia cores is a critical factor in the longevity of all-ceramic dental crowns and fixed dental prostheses. PMID:21802131

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

Nucleation, growth, and strain relaxation of lattice-mismatched 3-5 semiconductor epitaxial layers

NASA Technical Reports Server (NTRS)

Welser, R. E.; Guido, L. J.

1994-01-01

We have investigated the early stages of evolution of highly strained 2-D InAs layers and 3-D InAs islands grown by metal-organic chemical vapor deposition (MOCVD) on (100) and (111)B GaAs substrates. The InAs epilayer/GaAs substrate combination has been chosen because the lattice-mismatch is severe (approximately 7.2 percent), yet these materials are otherwise very similar. By examining InAs-on-GaAs composites instead of the more common In(x)Ga(1-x)As alloy we remove an additional degree of freedom (x) and thereby simplify data interpretation. A matrix of experiments is described in which the MOCVD growth parameters - susceptor temperature, Thin flux, and AsH3 flux - have been varied over a wide range. Scanning electron microscopy, atomic force microscopy, transmission electron microscopy, and electron microprobe analysis have been employed to observe the thin film surface morphology. In the case of 3-D growth, we have extracted activation energies and power-dependent exponents that characterize the nucleation process. As a consequence, optimized growth conditions have been identified for depositing approximately 250 A thick (100) and (111)B oriented InAs layers with relatively smooth surfaces. Together with preliminary data on the strain relaxation of these layers, the above results on the evolution of thin InAs films indicate that the (111)B orientation is particularly promising for yielding lattice-mismatched films that are fully relaxed with only misfit dislocations at the epilayer/substrate interface.

[Interface bond and compatibility between GI-II glass/alumina composite and Vitadur alpha veneering porcelain].

PubMed

Meng, Yukun; Chao, Yonglie; Liao, Yunmao

2002-01-01

Multiple layer techniques were commonly employed in fabricating all-ceramic restorations. Bond and compatibility between layers were vitally important for the clinical success of the restorations. The purposes of this study were to investigate the bond of the interface between the GI-II glass/alumina composite and Vitadur alpha veneering porcelain, and to study the thermal compatibility between them. Prepared a bar shaped specimen of GI-II glass/alumina composite 25 mm x 5 mm x 1 mm in size, with bottom surface pre-notched. The upper surface was veneered with Vitadur alpha veneering porcelain (0.2 mm opaque dentin and 0.6 mm dentin porcelain), then fractured and the fracture surface were examined under scanning electron microscope (SEM) and electron microprobe analyzer (EMPA) with electron beam of 10 micrometer in diameter; ten all-ceramic single crowns for an upper right central incisor were fabricated and the temperatures of thermal shock resistance were tested. SEM observation showed tight bond between the composite and the porcelain; The results of EMPA showed that penetration of Na, Al elements from glass/alumina into veneering porcelain and Si, K, Ca elements from veneering porcelain into glass/alumina occurred after sintering baking; The temperature of thermal shock resistance for anterior crowns in this study was 158 +/- 10.3 degrees C, cracks were mainly distributed in veneering porcelain with thicker layer. Chemical bond exists between the GI-II glass/alumina composite and Vitadur alpha veneering porcelain, and there is good thermal compatibility between them.

Spatial distribution of the RF power absorbed in a helicon plasma source

NASA Astrophysics Data System (ADS)

Aleksenko, O. V.; Miroshnichenko, V. I.; Mordik, S. N.

2014-08-01

The spatial distributions of the RF power absorbed by plasma electrons in an ion source operating in the helicon mode (ω ci < ω < ω ce < ω pe ) are studied numerically by using a simplified model of an RF plasma source in an external uniform magnetic field. The parameters of the source used in numerical simulations are determined by the necessity of the simultaneous excitation of two types of waves, helicons and Trivelpiece-Gould modes, for which the corresponding transparency diagrams are used. The numerical simulations are carried out for two values of the working gas (helium) pressure and two values of the discharge chamber length under the assumption that symmetric modes are excited. The parameters of the source correspond to those of the injector of the nuclear scanning microprobe operating at the Institute of Applied Physics, National Academy of Sciences of Ukraine. It is assumed that the mechanism of RF power absorption is based on the acceleration of plasma electrons in the field of a Trivelpiece-Gould mode, which is interrupted by pair collisions of plasma electrons with neutral atoms and ions of the working gas. The simulation results show that the total absorbed RF power at a fixed plasma density depends in a resonant manner on the magnetic field. The resonance is found to become smoother with increasing working gas pressure. The distributions of the absorbed RF power in the discharge chamber are presented. The achievable density of the extracted current is estimated using the Bohm criterion.

Auger electron spectroscopy at high spatial resolution and nA primary beam currents

NASA Technical Reports Server (NTRS)

Todd, G.; Poppa, H.; Moorhead, D.; Bales, M.

1975-01-01

An experimental Auger microprobe system is described which incorporates a field-emission electron gun and total beam currents in the nanoampere range. The distinguishing characteristics of this system include a large multistation UHV specimen chamber, pulse counting and fully digital Auger signal-processing techniques, and digital referencing methods to eliminate the effects of beam instabilities. Some preliminary results obtained with this system are described, and it is concluded that field-emission electron sources can be used for high-resolution Auger electron spectroscopy with primary-beam spots of less than 100 nm and beam currents of the order of 1 nA.

Classification of six ordinary chondrites from Texas

NASA Astrophysics Data System (ADS)

Ehlmann, Arthur J.; Keil, Klaus

1988-12-01

Based on optical microscopy, modal and electron microprobe analyses, six ordinary chondrites from Texas were classified in compositional groups, petrologic types, and shock facies. These meteorites are Comanche (stone), L5c; Haskell, L5c; Deport (a), H4b; Naruna (a), H4b; Naruna (b), H4b; and Clarendon (b), H5d.

Magnetic particles extracted from manganese nodules: Suggested origin from stony and iron meteorites

USGS Publications Warehouse

Finkelman, R.B.

1970-01-01

On the basis of x-ray diffraction and electron microprobe data, spherical and ellipsoidal particles extracted from manganese nodules were divided into three groups. Group I particles are believed to be derived from iron meteorites, and Group II particles from stony meteorites. Group III particles are believed to be volcanic in origin.

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.

Near-Field Scanning Optical Microscopy and Raman Microscopy.

NASA Astrophysics Data System (ADS)

Harootunian, Alec Tate

1987-09-01

Both a one dimensional near-field scanning optical microscope and Raman microprobe were constructed. In near -field scanning optical microscopy (NSOM) a subwavelength aperture is scanned in the near-field of the object. Radiation transmitted through the aperture is collected to form an image as the aperture scans over the object. The resolution of an NSOM system is essentially wavelength independent and is limited by the diameter of the aperture used to scan the object. NSOM was developed in an effort to provide a nondestructive in situ high spatial resolution probe while still utilizing photons at optical wavelengths. The Raman microprobe constructed provided vibrational Raman information with spatial resolution equivalent that of a conventional diffraction limited microscope. Both transmission studies and near-field diffration studies of subwavelength apertures were performed. Diffraction theories for a small aperture in an infinitely thin conducting screen, a slit in a thick conducting screen, and an aperture in a black screen were examined. All three theories indicate collimation of radiation to the size to the size of the subwavelength aperture or slit in the near-field. Theoretical calculations and experimental results indicate that light transmitted through subwavelength apertures is readily detectable. Light of wavelength 4579 (ANGSTROM) was transmitted through apertures with diameters as small as 300 (ANGSTROM). These studies indicate the feasibility of constructing an NSOM system. One dimensional transmission and fluorescence NSOM systems were constructed. Apertures in the tips of metallized glass pipettes width inner diameters of less than 1000 (ANGSTROM) were used as a light source in the NSOM system. A tunneling current was used to maintain the aperture position in the near-field. Fluorescence NSOM was demonstrated for the first time. Microspectroscopic and Raman microscopic studies of turtle cone oil droplets were performed. Both the Raman vibrational frequencies and the Raman excitation data indicate that the carotenoids are unaggregated. The carotenoid astaxanthin was identified in the orange and red droplets by Raman microscopy. Future applications for both Raman microscopy and near-field microscopy were proposed. Four methods of near-field distance regulation were also examined. Finally, theoretical exposure curves for near-field lithography were calculated. Both the near-field lithographic results and the near field diffraction studies indicate essentially wavelength independent resolution. (Abstract shortened with permission of author.).

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.

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.

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.

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.

Lime-pozzolana mortars in Roman catacombs: composition, structures and restoration

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

Sanchez-Moral, Sergio; Luque, Luis; Canaveras, Juan-Carlos

Analyses of microsamples collected from Roman catacombs and samples of lime-pozzolana mortars hardened in the laboratory display higher contents in carbonated binder than other subaerial Roman monuments. The measured environmental data inside the Saint Callistus and Domitilla catacombs show a constant temperature of 15-17 deg C, a high CO{sub 2} content (1700 to 3500 ppm) and a relative humidity close to 100%. These conditions and particularly the high CO{sub 2} concentration speed-up the lime calcitization roughly by 500% and reduce the cationic diffusion to form hydrous calcium aluminosilicates. The structure of Roman catacomb mortars shows (i) coarser aggregates and thickermore » beds on the inside, (ii) thin, smoothed, light and fine-grained external surfaces with low content of aggregates and (iii) paintings and frescoes on the outside. The observed high porosity of the mortars can be attributed to cracking after drying linked with the high binder content. Hardened lime lumps inside the binder denote low water/mortar ratios for slaking. The aggregate tephra pyroclasts rich in aluminosilicate phases with accessorial amounts of Ba, Sr, Rb, Cu and Pb were analysed through X-ray diffraction (XRD), electron microprobe analysis (EMPA) and also by environmental scanning electron microscopy (ESEM) to identify the size and distribution of porosity. Results support procedures using local materials, special mortars and classic techniques for restoration purposes in hypogeal backgrounds.« less

A study of hydrogen environment effects on microstructure property behavior of NASA-23 alloy and related alloy systems

NASA Technical Reports Server (NTRS)

Diwan, Ravinder M.

1990-01-01

This work is part of the overall advanced main combustion chamber (AMCC) casting characterization program of the Materials and Processes Laboratory of the Marshall Space Flight Center. The influence of hydrogen on the tensile properties and ductility behavior of NASA-23 alloy were analyzed. NASA-23 and other referenced alloys in cast and hipped conditions were solution treated and aged under selected conditions and characterized using optical metallography, scanning electron microscopy, and electron microprobe analysis techniques. The yield strength of NASA-23 is not affected much by hydrogen under tensile tests carried at 5000 psig conditions; however, the ultimate strength and ductility properties are degraded. This implies that the physical mechanisms operating would be related to the plastic deformation process. The fracture surfaces characteristics of NASA-23 specimens tensile tested in hydrogen, helium, and air were also analyzed. These revealed surface cracks around specimen periphery with the fracture surface showing a combination of intergranular and transgranular modes of fracture. It is seen that the specimens charged in hydrogen seem to favor a more brittle fracture mode in comparison to air and helium charged specimens. The AMCC casting characterization program is to be analyzed for their hydrogen behavior. As a result of this program, the basic microstructural factors and fracture characteristics in some cases were analyzed.

Techniques and Tools of NASA's Space Shuttle Columbia Accident Investigation

NASA Technical Reports Server (NTRS)

McDanels, Steve J.

2005-01-01

The Space Shuttle Columbia accident investigation was a fusion of many disciplines into a single effort. From the recovery and reconstruction of the debris, Figure 1, to the analysis, both destructive and nondestructive, of chemical and metallurgical samples, Figure 2, a multitude of analytical techniques and tools were employed. Destructive and non-destructive testing were utilized in tandem to determine if a breach in the left wing of the Orbiter had occurred, and if so, the path of the resultant high temperature plasma flow. Nondestructive analysis included topometric scanning, laser mapping, and real-time radiography. These techniques were useful in constructing a three dimensional virtual representation of the reconstruction project, specifically the left wing leading edge reinforced carbon/carbon heat protectant panels. Similarly, they were beneficial in determining where sampling should be performed on the debris. Analytic testing included such techniques as Energy Dispersive Electron Microprobe Analysis (EMPA), Electron Spectroscopy Chemical Analysis (ESCA), and X-Ray dot mapping; these techniques related the characteristics of intermetallics deposited on the leading edge of the left wing adjacent to the location of a suspected plasma breach during reentry. The methods and results of the various analyses, along with their implications into the accident, are discussed, along with the findings and recommendations of the Columbia Accident Investigation Board. Likewise, NASA's Return To Flight efforts are highlighted.

Mineralogical and chemical assessment of concrete damaged by the oxidation of sulfide-bearing aggregates: Importance of thaumasite formation on reaction mechanisms

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

Rodrigues, A.; Duchesne, J., E-mail: josee.duchesne@ggl.ulaval.ca; Fournier, B.

Damages in concrete containing sulfide-bearing aggregates were recently observed in the Trois-Rivieres area (Quebec, Canada), characterized by rapid deterioration within 3 to 5 years after construction. A petrographic examination of concrete core samples was carried out using a combination of tools including: stereomicroscopic evaluation, polarized light microscopy, scanning electron microscopy, X-ray diffraction and electron microprobe analysis. The aggregate used to produce concrete was an intrusive igneous rock with different metamorphism degrees and various proportions of sulfide minerals. In the rock, sulfide minerals were often surrounded by a thin layer of carbonate minerals (siderite). Secondary reaction products observed in the damagedmore » concrete include 'rust' mineral forms (e.g. ferric oxyhydroxides such as goethite, limonite (FeO (OH) nH{sub 2}O) and ferrihydrite), gypsum, ettringite and thaumasite. In the presence of water and oxygen, pyrrhotite oxidizes to form iron oxyhydroxides and sulphuric acid. The acid then reacts with the phases of the cement paste/aggregate and provokes the formation of sulfate minerals. Understanding both mechanisms, oxidation and internal sulfate attack, is important to be able to duplicate the damaging reaction in laboratory conditions, thus allowing the development of a performance test for evaluating the potential for deleterious expansion in concrete associated with sulfide-bearing aggregates.« less

Late-stage sulfides and sulfarsenides in Lower Cambrian black shale (stone coal) from the Huangjiawan mine, Guizhou Province, People's Republic of China

USGS Publications Warehouse

Belkin, H.E.; Luo, K.

2008-01-01

The Ni-Mo Huangjiawan mine, Guizhou Province, People's Republic of China, occurs in Lower Cambrian black shale (stone coal) in an area where other mines have recently extracted ore from the same horizon. Detailed electron microprobe (EMPA) and scanning electron microscope (SEM) analyses of representative thin sections have revealed a complex assemblage of sulfides and sulfarsenides. Early sulfidic and phosphatic nodules and host matrix have been lithified, somewhat fractured, and then mineralized with later-stage sulfides and sulfarsenides. Gersdorffite, millerite, polydymite, pyrite, sphalerite, chalcopyrite, galena, and clausthalite have been recognized. EMPA data are given for the major phases. Pyrite trace-element distributions and coeval Ni-, As-sulfides indicate that in the main ore layer, the last sulfide deposition was Ni-As-Co-rich. Mo and V deposition were early in the petrogenesis of these rocks. The assemblages gersdorffite-millerite-polydymite (pyrite) and millerite-gersdorffite (pyrite) and the composition of gersdorffite indicate a formation temperature of between 200?? and 300??C suggesting that the last solutions to infiltrate and mineralize the samples were related to hydrothermal processes. Environmentally sensitive elements such as As, Cd, and Se are hosted by sulfides and sulfarsenides and are the main source of these elements to residual soil. Crops grown on them are enriched in these elements, and they may be hazardous for animal and human consumption. ?? Springer-Verlag 2007.

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

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

A geochemical study of macerals from a Miocene lignite and an Eocene bituminous coal, Indonesia

USGS Publications Warehouse

Stankiewicz, B.A.; Kruge, M.A.; Mastalerz, Maria

1996-01-01

Optical and chemical studies of maceral concentrates from a Miocene lignite and an Eocene high-volatile bituminous C coal from southeastern Kalimantan, Indonesia were undertaken using pyro-Lysis, optical, electron microprobe and FTIR techniques Pyrolysis products of vitrinite from bituminous coal were dominated by straight-chain aliphatics and phenols. The huminite of the Miocene lignite produced mostly phenolic compounds upon pyrolysis. Differences in the pyrolysis products between the huminite and vitrinite samples reflect both maturation related and paleobotanical differences. An undefined aliphatic source and/or bacterial biomass were the likely contributors of n-alkyl moieties to the vitrinite. The resinite fraction in the lignite yielded dammar-derived pyrolysis products, as well as aliphatics and phenols as the products of admixed huminite and other liptinites. The optically defined resinite-rich fraction of the bituminous coal from Kalimantan produced abundant n-aliphatic moieties upon pyrolysis, but only two major resin markers (cadalene and 1,6-dimethylnaphthalene). This phenomenon is likely due to the fact that Eocene resins were not dammar-related. Data from the electron microprobe and Fourier transform infrared spectrometry strongly support the results obtained by Py GC MS and microscopy.

The onset of metamorphism in ordinary and carbonaceous chondrites

USGS Publications Warehouse

Grossman, J.N.; Brearley, A.J.

2005-01-01

Ordinary and carbonaceous chondrites of the lowest petrologic types were surveyed by X-ray mapping techniques. A variety of metamorphic effects were noted and subjected to detailed analysis using electron microprobe, scanning electron microscopy (SEM), transmission electron microscopy (TEM), and cathodoluminescence (CL) methods. The distribution of Cr in FeO-rich olivine systematically changes as metamorphism increases between type 3.0 and type 3.2. Igneous zoning patterns are replaced by complex ones and Cr-rich coatings develop on all grains. Cr distributions in olivine are controlled by the exsolution of a Cr-rich phase, probably chromite. Cr in olivine may have been partly present as tetrahedrally coordinated Cr3+. Separation of chromite is nearly complete by petrologic type 3.2. The abundance of chondrules showing an inhomogeneous distribution of alkalis in mesostasis also increases with petrologic type. TEM shows this to be the result of crystallization of albite. Residual glass compositions systematically change during metamorphism, becoming increasingly rich in K. Glass in type I chondrules also gains alkalis during metamorphism. Both types of chondrules were open to an exchange of alkalis with opaque matrix and other chondrules. The matrix in the least metamorphosed chondrites is rich in S and Na. The S is lost from the matrix at the earliest stages of metamorphism due to coalescence of minute grains. Progressive heating also results in the loss of sulfides from chondrule rims and increases sulfide abundances in coarse matrix assemblages as well as inside chondrules. Alkalis initially leave the matrix and enter chondrules during early metamorphism. Feldspar subsequently nucleates in the matrix and Na re-enters from chondrules. These metamorphic trends can be used to refine classification schemes for chondrites. Cr distributions in olivine are a highly effective tool for assigning petrologic types to the most primitive meteorites and can be used to subdivide types 3.0 and 3.1 into types 3.00 through 3.15. On this basis, the most primitive ordinary chondrite known is Semarkona, although even this meteorite has experienced a small amount of metamorphism. Allan Hills (ALH) A77307 is the least metamorphosed CO chondrite and shares many properties with the ungrouped carbonaceous chondrite Acfer 094. Analytical problems are significant for glasses in type II chondrules, as Na is easily lost during microprobe analysis. As a result, existing schemes for chondrule classification that are based on the alkali content of glasses need to be revised. ?? The Meteorological Society, 2005.

Scanning Electrochemical Microscopy as a Novel Proximity Sensor for Atraumatic Cochlear Implant Insertion

PubMed Central

Velmurugan, J.; Mirkin, M. V.; Svirsky, M. A.; Lalwani, A. K.; Llinas, R. R.

2014-01-01

A growing number of minimally invasive surgical and diagnostic procedures require the insertion of an optical, mechanical, or electronic device in narrow spaces inside a human body. In such procedures, precise motion control is essential to avoid damage to the patient’s tissues and/or the device itself. A typical example is the insertion of a cochlear implant which should ideally be done with minimum physical contact between the moving device and the cochlear canal walls or the basilar membrane. Because optical monitoring is not possible, alternative techniques for sub millimeter-scale distance control can be very useful for such procedures. The first requirement for distance control is distance sensing. We developed a novel approach to distance sensing based on the principles of scanning electrochemical microscopy (SECM). The SECM signal, i.e., the diffusion current to a microelectrode, is very sensitive to the distance between the probe surface and any electrically insulating object present in its proximity. With several amperometric microprobes fabricated on the surface of an insertable device, one can monitor the distances between different parts of the moving implant and the surrounding tissues. Unlike typical SECM experiments, in which a disk-shaped tip approaches a relatively smooth sample, complex geometries of the mobile device and its surroundings make distance sensing challenging. Additional issues include the possibility of electrode surface contamination in biological fluids and the requirement for a biologically compatible redox mediator. PMID:24845292

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.

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.

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.

Preliminary characterisation of new glass reference materials (GSA-1G, GSC-1G, GSD-1G and GSE-1G) by laser ablation-inductively coupled plasma-mass spectrometry using 193 nm, 213 nm and 266 nm wavelengths

USGS Publications Warehouse

Guillong, M.; Hametner, K.; Reusser, E.; Wilson, S.A.; Gunther, D.

2005-01-01

New glass reference materials GSA-1G, GSC-1G, GSD-1G and GSE-1G have been characterised using a prototype solid state laser ablation system capable of producing wavelengths of 193 nm, 213 nm and 266 nm. This system allowed comparison of the effects of different laser wavelengths under nearly identical ablation and ICP operating conditions. The wavelengths 213 nm and 266 nm were also used at higher energy densities to evaluate the influence of energy density on quantitative analysis. In addition, the glass reference materials were analysed using commercially available 266 nm Nd:YAG and 193 nm ArF excimer lasers. Laser ablation analysis was carried out using both single spot and scanning mode ablation. Using laser ablation ICP-MS, concentrations of fifty-eight elements were determined with external calibration to the NIST SRM 610 glass reference material. Instead of applying the more common internal standardisation procedure, the total concentration of all element oxide concentrations was normalised to 100%. Major element concentrations were compared with those determined by electron microprobe. In addition to NIST SRM 610 for external calibration, USGS BCR-2G was used as a more closely matrix-matched reference material in order to compare the effect of matrix-matched and non matrix-matched calibration on quantitative analysis. The results show that the various laser wavelengths and energy densities applied produced similar results, with the exception of scanning mode ablation at 266 nm without matrix-matched calibration where deviations up to 60% from the average were found. However, results acquired using a scanning mode with a matrix-matched calibration agreed with results obtained by spot analysis. The increased abundance of large particles produced when using a scanning ablation mode with NIST SRM 610, is responsible for elemental fractionation effects caused by incomplete vaporisation of large particles in the ICP.

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.

Petrographic and petrological study of lunar rock materials

NASA Technical Reports Server (NTRS)

Winzer, S. R.

1977-01-01

Impact melts and breccias from the Apollo 15 and 16 landing sites were examined optically and by electron microscope/microprobe. Major and trace element abundances were determined for selected samples. Apollo 16 breccias contained impact melts, metamorphic and primary igneous rocks. Metamorphic rocks may be the equivalents of the impact melts. Apollo 15 breccias studied were fragment-laden melts derived from gabbro and more basalt target rocks.

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.

Foliar manganese accumulation by Maytenus founieri (Celastraceae) in its native New Caledonian habitats: populational variation and localization by X-ray microanalysis.

PubMed

Fernando, D R; Woodrow, I E; Jaffré, T; Dumontet, V; Marshall, A T; Baker, A J M

2008-01-01

Hyperaccumulation by plants is a rare phenomenon that has potential practical benefits. The majority of manganese (Mn) hyperaccumulators discovered to date occur in New Caledonia, and little is known about their ecophysiology. This study reports on natural populations of one such species, the endemic shrub Maytenus founieri. Mean foliar Mn concentrations of two populations growing on ultramafic substrates with varying soil pHs were obtained. Leaf anatomies were examined by light microscopy, while the spatial distributions of foliar Mn in both populations were examined by qualitative scanning electron microscopy/energy dispersive spectroscopy (SEM/EDS). Plants growing on two different substrates were found to have very different mean dry weight (DW) foliar Mn concentrations. Light microscopy showed that the leaves had very distinct thick dermal structures, consisting of multiple layers of large cells in the hypodermis. In vivo X-ray microprobe analyses revealed that, in both populations, Mn sequestration occurred primarily in these dermal tissues. The finding here that foliar Mn is most highly localized in the nonphotosynthetic tissues of M. founieri contrasts with results from similar studies on other woody species that accumulate high Mn concentrations in their shoots.

Local melting in Al-Mg-Zn-alloys

NASA Astrophysics Data System (ADS)

Droenen, Per-Erik; Ryum, Nils

1994-03-01

The internal melting of several Al-Mg-Zn-alloys has been studied by rapid upquenching in a salt bath of specimens slowly cooled at a rate of 2 °C/h down to 375 °C. The melting reaction was studied metallographically in the light- and electron-scanning microscope, and local concentrations were measured in the microprobe. Local melting of both the equilibrium phases T and η was observed to occur. There were, however, essential differences between the melting kinetics for the two phases. While the T-phase particles melted spontaneously at temperatures at or above the invariant temperature, 489 °C, and after some period of time at lower temperatures, the η-phase particles either melted spontaneously at or above the invariant temperature, T - 475 °C, or dissolved into the matrix at temperatures below 475 °C. This difference in behavior can be accounted for if the α(Al)-η section is not a quasi-binary section. The industrial implications of the internal melting in these alloys are discussed and compared to the same reaction in the Al-Mg-Si alloys. A model is developed in the Appendix to quantify the different behaviors of these two classes of alloys.

Energetics of alkali and alkaline earth ion-exchanged zeolite A

DOE PAGES

Sun, Hui; Wu, Di; Liu, Kefeng; ...

2016-06-30

Alkali and alkaline earth ion-exchanged zeolite A samples were synthesized in aqueous exchange media. They were thoroughly studied by powder X-ray diffraction (XRD), electron microprobe (EMPA), thermogravimetric analysis and differential scanning calorimetry (TG-DSC), and high temperature oxide melt solution calorimetry. The hydration energetics and enthalpies of formation of these zeolite A materials from constituent oxides were determined. Specifically, the hydration level of zeolite A has a linear dependence on the average ionic potential ( Z/r) of the cation, from 0.894 (Rb-A) to 1.317 per TO 2 (Mg-A). The formation enthalpies from oxides (25 °C) range from –93.71 ± 1.77 (K-A)more » to –48.02 ± 1.85 kJ/mol per TO 2 (Li-A) for hydrated alkali ion-exchanged zeolite A, and from –47.99 ± 1.20 (Ba-A) to –26.41 ± 1.71 kJ/mol per TO 2 (Mg-A) for hydrated alkaline earth ion-exchanged zeolite A. As a result, the formation enthalpy from oxides generally becomes less exothermic as Z/r increases, but a distinct difference in slope is observed between the alkali and the alkaline earth series.« less

Investigation of the Geochemical Preservation of ca. 3.0 Ga Permineralized and Encapsulated Microfossils by Nanoscale Secondary Ion Mass Spectrometry

NASA Astrophysics Data System (ADS)

Delarue, Frédéric; Robert, François; Sugitani, Kenichiro; Tartèse, Romain; Duhamel, Rémi; Derenne, Sylvie

2017-12-01

Observations of Archean organic-walled microfossils suggest that their fossilization took place through both encapsulation and permineralization. In this study, we investigated microfossils from the ca. 3.0 Ga Farrel Quartzite (Pilbara, Western Australia) using transmitted light microscopy, scanning electron microscopy, Raman microspectrometry, and nanoscale secondary ion mass spectrometry (NanoSIMS) ion microprobe analyses. In contrast to previous studies, we demonstrated that permineralized microfossils were not characterized by the micrometric spatial relationships between Si and C-N as observed in thin sections. Permineralized microfossils are composed of carbonaceous globules that did not survive the acid treatment, whereas encapsulated microfossils were characterized due to their resistance to the acid maceration procedure. We also investigated the microscale relationship between the 12C14N- and 12C2- ion emission as a proxy of the N/C atomic ratio in both permineralized and encapsulated microfossils. After considering any potential matrix and microtopography effects, we demonstrate that the encapsulated microfossils exhibit the highest level of geochemical preservation. This finding shows that the chemical heterogeneity of the microfossils, observed at a spatial resolution of a few hundreds of micrometers, can be related to fossilization processes.

Diagenesis in coastal carbonates related to Pleistocene sea level, Bermuda Platform

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

Vollbrecht, R.; Meischner, D.

1996-01-01

Pleistocene glacioeustatic sea-level oscillation on the stable Bermuda Platform is expressed in a succession of shallow-water carbonates interrupted by lowstand unconformities. In Bermuda, the maximum highstands of the last 400,000 yr ranged within 10 m around the present level. Coastal carbonates of various highstands are exposed along the present shoreline. These carbonates were penetrated by meteoric and marine pore waters during lowstands and highstands following on deposition. Two representative Pleistocene shoreline sections were studied to see whether early diagenesis has recorded these pore-water changes. The sediments of both sections show multiple generations of cement. Optical and scanning electron microscopy, cathodoluminescencemore » microscopy, X-ray diffraction, microprobe studies and stable-isotope analyses were used to determine the diagenetic environments involved. Regardless of the degree of substrate cementation, freshwater alteration was mainly vadose whereas marine cementation was either phreatic or vadose or both. Early diagenetic oscillation is easier recorded in coastal successions than in lagoonal sediments, mainly because marine cementation is more active nearshore.Because the coastal environment is prone to wave destruction, the potential for preserving these diagenetic features is usually low. Data published on tectonically unstable areas suggest that early diagenetic oscillation may characterize stable coastlines.« 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.

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

USGS Publications Warehouse

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

1962-01-01

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

Determination of niobium in rocks, ores and alloys by atomic-absorption spectrophotometry.

PubMed

Husler, J

1972-07-01

Niobium, in concentrations as low as 0.02% Nb(2)O(5), is determined in a variety of materials without separation or enrichment. Chemical and ionization interferences are controlled, and sensitivity is increased, by maintaining the iron, aluminium, hydrofluoric acid and potassium content within certain broad concentration limits. There is close agreement with the results of analyses by emission spectrographic, electron microprobe and X-ray fluorescence methods.

Investigation of gold embrittlement in connector solder joints

NASA Technical Reports Server (NTRS)

Lane, F. L.

1972-01-01

An investigation was performed to determine to what extent typical flight connector solder joints may be embrittled by the presence of gold. In addition to mapping of gold content in connector solder joints by an electron microprobe analyzer, metallographic examinations and mechanical tests (thermal shock, vibration, impact and tensile strength) were also conducted. A description of the specimens and tests, a discussion of the data, and some conclusions are presented.

Mineral precipitation and dissolution at two slag-disposal sites in northwestern Indiana, USA

USGS Publications Warehouse

Bayless, E.R.; Schulz, M.S.

2003-01-01

Slag is a ubiquitous byproduct of the iron- and steel-refining industries. In northwestern Indiana and northeastern Illinois, slag has been deposited over more than 52 km2 of land surface. Despite the widespread use of slag for fill and construction purposes, little is known about its chemical effects on the environment. Two slagdisposal sites were examined in northwestern Indiana where slag was deposited over the native glacial deposits. At a third site, where slag was not present, background conditions were defined. Samples were collected from cores and drill cuttings and described with scanning electron microscopy and electron microprobe analysis. Ground-water samples were collected and used to assess thermodynamic equilibria between authigenic minerals and existing conditions. Differences in the mineralogy at background and slag-affected sites were apparent. Calcite, dolomite, gypsum, iron oxides, and clay minerals were abundant in native sediments immediately beneath the slag. Mineral features indicated that these minerals precipitated rapidly from slag drainage and co-precipitated minor amounts of non-calcium metals and trace elements. Quartz fragments immediately beneath the slag showed extensive pitting that was not apparent in sediments from the background site, indicating chemical weathering by the hyperalkaline slag drainage. The environmental impacts of slag-related mineral precipitation include disruption of natural ground-water flow patterns and bed-sediment armoring in adjacent surface-water systems. Dissolution of native quartz by the hyperalkaline drainage may cause instability in structures situated over slag fill or in roadways comprised of slag aggregates.

Thermoelectric Inhomogeneities in (Ag(sub 1-y)SbTe2)(sub x)(PbTe)(sub 1-x)

NASA Technical Reports Server (NTRS)

Snyder, G. Jeffrey; Chen, Nancy; Gascoin, Franck; Mueller, Eckhard; Karpinski, Gabriele; Stiewe, Christian

2006-01-01

A document presents a study of why materials of composition (Ag1 ySbTe2)0.05 (PbTe)0.95 [0< or = y < or = 1] were previously reported to have values of the thermoelectric figure of merit [ZT (where Z = alpha(sup 2)/rk, alpha is the Seebeck coefficient, r is electrical resistivity, k is thermal conductivity, and T is absolute temperature)] ranging from <1 to >2. In the study, samples of (AgSbTe2)0.05(PbTe)0.95, (Ag0.67SbTe2)0.05 (PbTe)0.95, and (Ag0.55SbTe2)0.05(PbTe)0.95 were prepared by melting followed, variously, by slow or rapid cooling. Analyses of these samples by x-ray diffraction, electron microscopy, and scanning-microprobe measurements of the Seebeck coefficient led to the conclusion that these materials have a multiphase character on a scale of the order of millimeters, even though they appear homogeneous in x-ray diffraction and electron microscopy. The Seebeck measurements showed significant variations, including both n-type and p-type behavior in the same sample. These variations were found to be consistent with observed variations of ZT. The rapidly quenched samples were found to be less inhomogeneous than were the furnace-cooled ones; hence, rapid quenching was suggested as a basis of research on synthesizing more nearly uniform high-ZT samples.

Fe/Mg smectite formation under acidic conditions on early Mars

NASA Astrophysics Data System (ADS)

Peretyazhko, T. S.; Sutter, B.; Morris, R. V.; Agresti, D. G.; Le, L.; Ming, D. W.

2016-01-01

Phyllosilicates of the smectite group detected in Noachian and early Hesperian terrains on Mars have been hypothesized to form under neutral to alkaline conditions. These pH conditions would also be favorable for formation of widespread carbonate deposits which have not been detected on Mars. We propose that smectite deposits on Mars formed under moderately acidic conditions inhibiting carbonate formation. We report here the first synthesis of Fe/Mg smectite in an acidic hydrothermal system [200 °C, pHRT ∼ 4 (pH measured at room temperature) buffered with acetic acid] from Mars-analogue, glass-rich, basalt simulant with and without aqueous Mg or Fe(II) addition under N2-purged anoxic and ambient oxic redox conditions. Synthesized Fe/Mg smectite was examined by X-ray-diffraction, Mössbauer spectroscopy, visible and near-infrared reflectance spectroscopy, scanning electron microscopy and electron microprobe to characterize mineralogy, morphology and chemical composition. Alteration of the glass phase of basalt simulant resulted in formation of the Fe/Mg smectite mineral saponite with some mineralogical and chemical properties similar to the properties reported for Fe/Mg smectite on Mars. Our experiments are evidence that neutral to alkaline conditions on early Mars are not necessary for Fe/Mg smectite formation as previously inferred. Phyllosilicate minerals could instead have formed under mildly acidic pH conditions. Volcanic SO2 emanation and sulfuric acid formation is proposed as the major source of acidity for the alteration of basaltic materials and subsequent formation of Fe/Mg smectite.

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

High-MgO Vitric Ash in Upper Kulanaokuaiki Tephra, Kilauea Volcano, Hawai`i: A Preliminary Description

NASA Astrophysics Data System (ADS)

Rose, T. R.; Fiske, R. S.; Swanson, D.

2011-12-01

Small, well-formed Pele's tears containing anomalously high values of MgO were recently discovered in outcrops of the upper Kulanaokuaiki Tephra at and near the base of Uwekahuna Bluff, the western wall of Kilauea Caldera. Electron microprobe analyses of more than 60 high-MgO tears, which are 1-3 mm in diameter, show that most contain 11 to 12 wt. % MgO with a few approaching 13 % MgO. Separate microprobe analyses for sulfur and chlorine of 20 grains revealed no appreciable amounts of either, indicating the magma was largely degassed. Polished-section studies employing an analytical scanning electron microscope show most tears are composed of pure microvesicular glass with scattered skeletal olivine crystals and rare chromite. The abundance of skeletal olivine appears to increase with decreasing MgO content of the glass. These tears contain among the highest known MgO values of any material erupted subaerially from Kilauea. The high-MgO tears occur in a 1-6 cm thick layer of medium-coarse lithic-crystal-vitric ash. The top of this layer consists of 2-3 mm of very fine lithic-crystal ash. The lithics and many of the olivine crystals in this layer are highly oxidized. This deposit is at the top of a sequence of several lithic beds that are interspersed with thinner vitric units totaling about 75 cm in thickness. It is overlain by 9-13 cm of medium pumice lapilli and coarse vitric ash at the top of the "Bluff base" and "mid-Bluff" tephra sections described by Fiske et al. (2009). This high-MgO glass layer has been found thus far in only one other locality, a 2 m-deep soils study pit within Kipuka Puaulu, 3.5 km northwest of the caldera. Based upon stratigraphic relationships and preliminary microprobe data, a few other likely exposures of the high-MgO deposit have been identified north and west of the caldera. The high-MgO vitric ash in the upper Kulanaokuaiki Tephra has a primitive composition that suggests little if any shallow level storage of magma. Instead, the magma probably rose rapidly from deep within, or below, the volcano just before its eruption. Remnants of the Kulanaokuaiki-3 scoria deposit, a subunit of the upper Kulanaokuaiki Tephra, are preserved over wide areas 7-12 km south and southeast of the summit and have characteristics also suggesting rapid rise and eruption (Fiske et al., this meeting). Some relatively primitive vitric ash occurs in the younger Keanakako`i Tephra (Garcia et al., this meeting) and can be interpreted to indicate little if any shallow storage. Thus the high-MgO glass reported here may be an end member in a family of relatively primitive compositions that can erupt under some circumstances at Kilauea's summit. Most recent tephra deposits at and near Kilauea's summit are attributed to phreatic or phreatomagmatic explosive eruptions that originated at relatively shallow depth. One important implication of our findings is that some highly energetic pyroclastic eruptions at Kilauea likely originated at far greater depths.

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.

New techniques for imaging and analyzing lung tissue.

PubMed Central

Roggli, V L; Ingram, P; Linton, R W; Gutknecht, W F; Mastin, P; Shelburne, J D

1984-01-01

The recent technological revolution in the field of imaging techniques has provided pathologists and toxicologists with an expanding repertoire of analytical techniques for studying the interaction between the lung and the various exogenous materials to which it is exposed. Analytical problems requiring elemental sensitivity or specificity beyond the range of that offered by conventional scanning electron microscopy and energy dispersive X-ray analysis are particularly appropriate for the application of these newer techniques. Electron energy loss spectrometry, Auger electron spectroscopy, secondary ion mass spectrometry, and laser microprobe mass analysis each offer unique advantages in this regard, but also possess their own limitations and disadvantages. Diffraction techniques provide crystalline structural information available through no other means. Bulk chemical techniques provide useful cross-checks on the data obtained by microanalytical approaches. It is the purpose of this review to summarize the methodology of these techniques, acknowledge situations in which they have been used in addressing problems in pulmonary toxicology, and comment on the relative advantages and disadvantages of each approach. It is necessary for an investigator to weigh each of these factors when deciding which technique is best suited for any given analytical problem; often it is useful to employ a combination of two or more of the techniques discussed. It is anticipated that there will be increasing utilization of these technologies for problems in pulmonary toxicology in the decades to come. Images FIGURE 3. A FIGURE 3. B FIGURE 3. C FIGURE 3. D FIGURE 4. FIGURE 5. FIGURE 7. A FIGURE 7. B FIGURE 8. A FIGURE 8. B FIGURE 8. C FIGURE 9. A FIGURE 9. B FIGURE 10. PMID:6090115

The Hollow Spheres of the Orgueil Meteorite: A Re-Examination

NASA Technical Reports Server (NTRS)

Hoover, Richard B.; Jerman, Gregory; Rossignold-Strick, Maritine

2005-01-01

In 1971, Rossignol-Strick and Barghoorn provided images and a description of a number of spherical hollow microstructures showing well-defined walls in acid macerated extract of the Orgueil CI carbonaceous meteorite. Other forms such as membranes and spiral shaped structures were also reported. The carbon-rich (kerogen) hollow spheres were found to be in a narrowly constrained distribution of sizes (mainly 7 to 10 microns in diameter). Electron microprobe analysis revealed that these spheres contained Carbon, possibly P, N, and K. It was established that these forms could not be attributed to pollen or other recent terrestrial contaminants. It was concluded that they most probably represented organic coatings on globules of glass, olivine or magnetite in the meteorite. However, recent studies of the Orgueil meteorite have been carried out at the NASA/Marshall Space Flight Center with the S-4000 Hitachi Field Emission Scanning Electron Microscope (FESEM). These investigations have revealed the presence of numerous carbon encrusted spherical magnetite platelets and spherical and ovoidal bodies of elemental iron in-situ in freshly fractured interior surfaces of the meteorite. Their size range is also very narrowly constrained (typically approximately 6 to 12 microns) in diameter. High resolution images reveal that these bodies are also encrusted with a thin carbonaceous sheath and are surrounded by short nanofibrils that are shown to be composed of high purity iron by EDAX elemental analysis. We present Secondary and Backscatter Electron FESEM images and associated EDAX elemental analyses and 2D X-ray maps of these forms as we re-examine the hollow spheres of Orgueil and attempt to determine if they are representatives of the same population of indigenous microstructures.

Application of High-Throughput Seebeck Microprobe Measurements on Thermoelectric Half-Heusler Thin Film Combinatorial Material Libraries.

PubMed

Ziolkowski, Pawel; Wambach, Matthias; Ludwig, Alfred; Mueller, Eckhard

2018-01-08

In view of the variety and complexity of thermoelectric (TE) material systems, combinatorial approaches to materials development come to the fore for identifying new promising compounds. The success of this approach is related to the availability and reliability of high-throughput characterization methods for identifying interrelations between materials structures and properties within the composition spread libraries. A meaningful characterization starts with determination of the Seebeck coefficient as a major feature of TE materials. Its measurement, and hence the accuracy and detectability of promising material compositions, may be strongly affected by thermal and electrical measurement conditions. This work illustrates the interrelated effects of the substrate material, the layer thickness, and spatial property distributions of thin film composition spread libraries, which are studied experimentally by local thermopower scans by means of the Potential and Seebeck Microprobe (PSM). The study is complemented by numerical evaluation. Material libraries of the half-Heusler compound system Ti-Ni-Sn were deposited on selected substrates (Si, AlN, Al 2 O 3 ) by magnetron sputtering. Assuming homogeneous properties of a film, significant decrease of the detected thermopower S m can be expected on substrates with higher thermal conductivity, yielding an underestimation of materials thermopower between 15% and 50%, according to FEM (finite element methods) simulations. Thermally poor conducting substrates provide a better accuracy with thermopower underestimates lower than 8%, but suffer from a lower spatial resolution. According to FEM simulations, local scanning of sharp thermopower peaks on lowly conductive substrates is linked to an additional deviation of the measured thermopower of up to 70% compared to homogeneous films, which is 66% higher than for corresponding cases on substrates with higher thermal conductivity of this study.

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

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

Speciation and characterization of arsenic in gold ores and cyanidation tailings using X-ray absorption spectroscopy

USGS Publications Warehouse

Paktunc, D.; Foster, A.; Heald, S.; Laflamme, G.

2004-01-01

The knowledge of mineralogy and molecular structure of As is needed to better understand the stability of As in wastes resulting from processing of gold ores. In this study, optical microscopy, scanning electron microscopy, electron microprobe, X-ray diffraction and X-ray absorption fine structure (XAFS) spectroscopy (including both XANES and EXAFS regimes) were employed to determine the mineralogical composition and local coordination environment of As in gold ores and process tailings from bench-scale tests designed to mimic a common plant practice. Arsenic-bearing minerals identified in the ores and tailings include iron (III) oxyhydroxides, scorodite (FeAsO4??2H2O), ferric arsenates, arseniosiderite (Ca2Fe3 (AsO4)3O2??3H2O), Ca-Fe arsenates, pharmacosiderite (KFe4 (AsO4)3(OH)4??6-7H2O), jarosite (K2Fe6(SO4)4 (OH)12) and arsenopyrite (FeAsS). Iron (III) oxyhydroxides contain variable levels of As from trace to about 22 wt% and Ca up to approximately 9 wt%. Finely ground ore and tailings samples were examined by bulk XAFS and selected mineral grains were analyzed by microfocused XAFS (micro-EXAFS) spectroscopy to reconcile the ambiguities of multiple As sources in the complex bulk EXAFS spectra. XANES spectra indicated that As occurs as As5+in all the samples. Micro-EXAFS spectra of individual iron (III) oxyhydroxide grains with varying As concentrations point to inner-sphere bidentate-binuclear arsenate complexes as the predominant form of As. There are indications for the presence of a second Fe shell corresponding to bidentate-mononuclear arrangement. Iron (III) oxyhydroxides with high As concentrations corresponding to maximum adsorption densities probably occur as nanoparticles. The discovery of Ca atoms around As in iron (III) oxyhydroxides at interatomic distances of 4.14-4.17 A?? and the coordination numbers suggest the formation of arseniosiderite-like nanoclusters by coprecipitation rather than simple adsorption of Ca onto iron (III) oxyhydroxides. Correlation of Ca with As in iron (III) oxyhydroxides as determined by electron microprobe analysis supports the coprecipitate origin for the presence of Ca in iron (III) oxyhydroxides. The samples containing higher abundances of ferric arsenates released higher As concentrations during the cyanidation tests. The presence of highly soluble ferric arsenates and Ca-Fe arsenates, and relatively unstable iron (III) oxyhydroxides with Fe/As molar ratios of less than 4 in the ore and process tailings suggests that not only the tailings in the impoundment will continue to release As, but also there is the potential for mobilization of As from the natural sources such as the unmined ore. ?? 2004 Elsevier Ltd.

Speciation and characterization of arsenic in gold ores and cyanidation tailings using X-ray absorption spectroscopy

NASA Astrophysics Data System (ADS)

Paktunc, Dogan; Foster, Andrea; Heald, Steve; Laflamme, Gilles

2004-03-01

The knowledge of mineralogy and molecular structure of As is needed to better understand the stability of As in wastes resulting from processing of gold ores. In this study, optical microscopy, scanning electron microscopy, electron microprobe, X-ray diffraction and X-ray absorption fine structure (XAFS) spectroscopy (including both XANES and EXAFS regimes) were employed to determine the mineralogical composition and local coordination environment of As in gold ores and process tailings from bench-scale tests designed to mimic a common plant practice. Arsenic-bearing minerals identified in the ores and tailings include iron (III) oxyhydroxides, scorodite (FeAsO 4·2H 2O), ferric arsenates, arseniosiderite (Ca 2Fe 3(AsO 4) 3O 2·3H 2O), Ca-Fe arsenates, pharmacosiderite (KFe 4(AsO 4) 3(OH) 4·6-7H 2O), jarosite (K 2Fe 6(SO 4) 4(OH) 12) and arsenopyrite (FeAsS). Iron (III) oxyhydroxides contain variable levels of As from trace to about 22 wt% and Ca up to approximately 9 wt%. Finely ground ore and tailings samples were examined by bulk XAFS and selected mineral grains were analyzed by microfocused XAFS (micro-EXAFS) spectroscopy to reconcile the ambiguities of multiple As sources in the complex bulk EXAFS spectra. XANES spectra indicated that As occurs as As 5+in all the samples. Micro-EXAFS spectra of individual iron (III) oxyhydroxide grains with varying As concentrations point to inner-sphere bidentate-binuclear arsenate complexes as the predominant form of As. There are indications for the presence of a second Fe shell corresponding to bidentate-mononuclear arrangement. Iron (III) oxyhydroxides with high As concentrations corresponding to maximum adsorption densities probably occur as nanoparticles. The discovery of Ca atoms around As in iron (III) oxyhydroxides at interatomic distances of 4.14-4.17 Å and the coordination numbers suggest the formation of arseniosiderite-like nanoclusters by coprecipitation rather than simple adsorption of Ca onto iron (III) oxyhydroxides. Correlation of Ca with As in iron (III) oxyhydroxides as determined by electron microprobe analysis supports the coprecipitate origin for the presence of Ca in iron (III) oxyhydroxides. The samples containing higher abundances of ferric arsenates released higher As concentrations during the cyanidation tests. The presence of highly soluble ferric arsenates and Ca-Fe arsenates, and relatively unstable iron (III) oxyhydroxides with Fe/As molar ratios of less than 4 in the ore and process tailings suggests that not only the tailings in the impoundment will continue to release As, but also there is the potential for mobilization of As from the natural sources such as the unmined ore.

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

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.

Raman spectroscopy as a tool to characterize heterogenite (CoO·OH) (Katanga Province, Democratic Republic of Congo)

NASA Astrophysics Data System (ADS)

Burlet, C.; Vanbrabant, Y.; Goethals, H.; Thys, T.; Dupin, L.

2011-10-01

Natural heterogenite (CoO·OH) samples were studied by Raman microspectroscopy, electronic microprobe and Electronic BackScattered Diffraction (EBSD). Raw samples and polished sections were made from 10 mines covering the Katanga copperbelt (Katanga Province, Democratic Republic of Congo). Four typical Raman responses have been obtained leading to investigate the laser-induced dehydroxylation of heterogenite into a Co-spinel structure. The results are also compared with EBSD patterns from oven heated heterogenite samples. A close relationship was established between the chemical substitutions of Co by mainly Cu, Ni, Mn and Al and their impact on the mineral Raman response.

Microscale reconstruction of biogeochemical substrates using multimode X-ray tomography and scanning electron microscopy

NASA Astrophysics Data System (ADS)

Miller, M.; Miller, E.; Liu, J.; Lund, R. M.; McKinley, J. P.

2012-12-01

X-ray computed tomography (CT), scanning electron microscopy (SEM), electron microprobe analysis (EMP), and computational image analysis are mature technologies used in many disciplines. Cross-discipline combination of these imaging and image-analysis technologies is the focus of this research, which uses laboratory and light-source resources in an iterative approach. The objective is to produce images across length scales, taking advantage of instrumentation that is optimized for each scale, and to unify them into a single compositional reconstruction. Initially, CT images will be collected using both x-ray absorption and differential phase contrast modes. The imaged sample will then be physically sectioned and the exposed surfaces imaged and characterized via SEM/EMP. The voxel slice corresponding to the physical sample surface will be isolated computationally, and the volumetric data will be combined with two-dimensional SEM images along CT image planes. This registration step will take advantage of the similarity between the X-ray absorption (CT) and backscattered electron (SEM) coefficients (both proportional to average atomic number in the interrogated volume) as well as the images' mutual information. Elemental and solid-phase distributions on the exposed surfaces, co-registered with SEM images, will be mapped using EMP. The solid-phase distribution will be propagated into three-dimensional space using computational methods relying on the estimation of compositional distributions derived from the CT data. If necessary, solid-phase and pore-space boundaries will be resolved using X-ray differential phase contrast tomography, x-ray fluorescence tomography, and absorption-edge microtomography at a light-source facility. Computational methods will be developed to register and model images collected over varying scales and data types. Image resolution, physically and dynamically, is qualitatively different for the electron microscopy and CT methodologies. Routine CT images are resolved at 10-20 μm, while SEM images are resolved at 10-20 nm; grayscale values vary according to collection time and instrument sensitivity; and compositional sensitivities via EMP vary in interrogation volume and scale. We have so far successfully registered SEM imagery within a multimode tomographic volume and have used standard methods to isolate pore space within the volume. We are developing a three-dimensional solid-phase identification and registration method that is constrained by bulk-sample X-ray diffraction Rietveld refinements. The results of this project will prove useful in fields that require the fine-scale definition of solid-phase distributions and relationships, and could replace more inefficient methods for making these estimations.

Trace Element Abundance Measurements on Cosmic Dust Particles

NASA Technical Reports Server (NTRS)

Flynn, George

1996-01-01

The X-Ray Microprobe on beamline X-26A at the National Synchrotron Light Source (NSLS) at Brookhaven National Laboratory was used to determine the abundances of elements from Cr through Sr in individual interplanetary dust particles (IDPs) collected from the Earth's stratosphere and the Scanning Transmission X-ray Microscope (STXM) on beamline X-1A at the NSLS was used to determine the carbon abundances and spatial distributions in IDPs. In addition, modeling was performed in an attempt to associate particular types of IDPs with specific types of parent bodies, and thus to infer the chemistry, mineralogy, and structural properties of those parent bodies.

Mercury Cadmium Telluride Sputtering Research.

DTIC Science & Technology

1982-08-28

originally designed for 5.7cm rather than 12.7cu diameter targets. A similar target made from poly- crystalline (Hg.8 Cd.2)Te material, which is difficult to...required 3 stainless steel pieces per dit, but provded a loM thamrl idauce for the diemspated taret power. The details of the design re given in...analyzed: 2) WDX detects and measures only one element at a time thereby ensuring better accuracy; 3) Since WDX electron microprobe is especially designed

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.

Genesis of highland basalt breccias - A view from 66095

NASA Technical Reports Server (NTRS)

Garrison, J. R., Jr.; Taylor, L. A.

1980-01-01

Electron microprobe and defocused beam analyses of the lunar highland breccia sample 66095 show it consists of a fine-grained subophitic matrix containing a variety of mineral and lithic clasts, such as intergranular and cataclastic ANT, shocked and unshocked plagioclase, and basalts. Consideration of the chemistries of both matrix and clasts provides a basis for a qualitative three-component mixing model consisting of an ANT plutonic complex, a Fra Mauro basalt, and minor meteoric material.

Stabilized phosphogypsum: class C fly ash: Portland type II cement composites for potential marine application.

PubMed

Guo, T; Malone, R F; Rusch, K A

2001-10-01

Phosphogypsum (PG, CaSO4 x H20), a byproduct of phosphoric acid manufacturing, contains low levels of Ra226. PG can be stabilized with portland type II cement and class C fly ash for use in marine environments, thus eliminating the airborne vector of transmission for radon gas. An augmented simplex centroid design with pseudocomponents was used to select 10 PG:class C fly ash:portland type II cement compositions. The 43 cm3 blocks were fabricated and subjected to a 1.5-yr field submergence test and a 28-d saltwater dynamic leaching study. All field composites survived with no signs of degradation. Dynamic leaching resulted in effective calcium diffusion coefficients ranging from 0.21 to 7.5 x 10(-14)m2 s(-1). Effective diffusion depths, calculated for t=1 and 30 yr, ranged from 0.4 to 2.2 mm and from 2.0 to 11.9 mm, respectively. Scanning electron microscopy and wavelength dispersive microprobe and X-ray diffraction analyses of the leached composites identified a 40-60-microm calcite layer that was absent in the control composites. This suggests that a reaction between the composites and the saltwater results in the precipitation of calcite onto the block surface, encapsulating the composites and protecting them from saltwater attack and dissolution.

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.

Application of a nuclear microprobe to the study of calcified tissues

NASA Astrophysics Data System (ADS)

Coote, Graeme E.; Vickridge, Ian C.

1988-03-01

The mineral fraction of calcified tissue is largely calcium hydroxyapatite (bones and teeth) or calcium carbonate (shells and fish otoliths). Apatite has such a strong affinity for fluoride ions that the F/Ca ratio can vary markedly with position in a bone or tooth, depending on the amount of fluoride present at the time of calcification or partial recrystallization. New biological information can be obtained by introducing extra fluoride into the diet of an animal and using a microprobe later to scan sections of bones or teeth. In suitable burial sites extra fluoride is introduced after death, and the new distribution may have applications in forensic science and archaeology. Fish otoliths are also of interest since a new carbonate layer is formed each day and the distribution of trace elements may record some aspects of the fish's life history. Results from the following studies are presented: fluorine distributions in the teeth of sheep which ingested extra fluoride for known periods; distributions of calcium and fluorine in femurs of rats which drank water high in fluoride for periods from 2 to 15 weeks; calcium and fluorine distributions in artificially-prepared lesions in tooth enamel; diffusion profiles in archaeological human teeth and animal bones; patterns in the strontium/calcium ratio in sectioned otoliths of several species of fish.

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.

Ion and laser microprobes applied to the measurement of corrosion produced hydrogen on a microscopic scale.

NASA Technical Reports Server (NTRS)

Gray, H. R.

1972-01-01

Use of an ion microprobe and a laser microprobe to measure concentrations of corrosion-produced hydrogen on a microscopic scale. Hydrogen concentrations of several thousand ppm were measured by both analytical techniques below corroded and fracture surfaces of hot salt stress corroded titanium alloy specimens. This extremely high concentration compares with only about 100 ppm hydrogen determined by standard vacuum fusion chemical analyses of bulk samples. Both the ion and laser microprobes were used to measure hydrogen concentration profiles in stepped intervals to substantial depths below the original corroded and fracture surfaces. For the ion microprobe, the area of local analysis was 22 microns in diameter and for the laser microprobe, the area of local analysis was about 300 microns in diameter. The segregation of hydrogen below fracture surfaces supports a previously proposed theory that corrosion-produced hydrogen is responsible for hot salt stress corrosion embrittlement and cracking of titanium alloys. These advanced analytical techniques suggest great potential for many areas of stress corrosion and hydrogen embrittlement research, quality control, and field inspection of corrosion problems. For example, it appears possible that a contour map of hydrogen distribution at notch roots and crack tips could be quantitatively determined. Such information would be useful in substantiating current theories of stress corrosion and hydrogen embrittlement.

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.

Effects of Chlorine Promoted Oxidation on Arsenic Release from Sulfide Minerals

NASA Astrophysics Data System (ADS)

West, N.; Schreiber, M.; Gotkowitz, M.

2007-12-01

High arsenic concentrations (>100 ppb) have been measured in wells completed in the Ordovician St. Peter sandstone aquifer of eastern Wisconsin. The primary source of arsenic is As-bearing sulfide minerals within the aquifer. Periodic disinfection of wells by chlorination may facilitate arsenic release to groundwater by increasing the rate of sulfide mineral oxidation. During typical well disinfection procedures, aquifer solids exposed along uncased portions of wells remain in direct contact with chlorine disinfection solutions for up to twenty-four hours. Due to the redox sensitivity of arsenic mobility in groundwater, it is important to evaluate the effect of repeatedly adding oxidizers to an arsenic impacted aquifer system. This study focuses on abiotic processes that mobilize arsenic from the solid phase during controlled exposure to chlorinated solutions. Two St. Peter samples with As concentrations of 21 and 674 ppm were selected for the experiments. Before reaction, the aquifer mineralogy is characterized using scanning electron microscopy (SEM) and electron microprobe analysis (EMPA). The samples are then reacted with solutions of 60 mg/L free chlorine, 1200 mg/L free chlorine, or nanopure water (control) at pH 7.0 and pH 8.5. These parameters represent typical solution chemistries present within the wells after disinfection. Solutions are sampled periodically during the experiments and analyzed for As, Fe, other trace metals such as Co, Mo, Cr, and Ni, and sulfate. Analysis of the post-reaction solids using SEM, EMPA, laser ablation ICP-MS and Raman techniques are used to document the changes in mineralogy due to chlorination and to document which solid phases contain As.

Titanospirillum velox: a huge, speedy, sulfur-storing spirillum from Ebro Delta microbial mats

NASA Technical Reports Server (NTRS)

Guerrero, R.; Haselton, A.; Sole, M.; Wier, A.; Margulis, L.

1999-01-01

A long (20-30 micrometer), wide (3-5 micrometer) microbial-mat bacterium from the Ebro Delta (Tarragona, Spain) was grown in mixed culture and videographed live. Intracellular elemental sulfur globules and unique cell termini were observed in scanning-electron-microprobe and transmission-electron micrographs. A polar organelle underlies bundles of greater than 60 flagella at each indented terminus. These Gram-negative bacteria bend, flex, and swim in a spiral fashion; they translate at speeds greater than 10 body lengths per second. The large size of the spirillum permits direct observation of cell motility in single individual bacteria. After desiccation (i.e., absence of standing water for at least 24 h), large populations developed in mat samples remoistened with sea water. Ultrastructural observations reveal abundant large sulfur globules irregularly distributed in the cytoplasm. A multilayered cell wall, pliable and elastic yet rigid, distends around the sulfur globules. Details of the wall, multiflagellated termini, and large cytoplasmic sulfur globules indicate that these fast-moving spirilla are distinctive enough to warrant a genus and species designation: Titanospirillum velox genus nov., sp. nov. The same collection techniques at a similar habitat in the United States (Plum Island, northeast Essex County, Massachusetts) also yielded large populations of the bacterium among purple phototrophic and other inhabitants of sulfurous microbial-mat muds. The months-long survival of T. velox from Spain and from the United States in closed jars filled with mud taken from both localities leads us to infer that this large spirillum has a cosmopolitan distribution.

Characteristics and origin of the relatively high-quality tight reservoir in the Silurian Xiaoheba Formation in the southeastern Sichuan Basin

PubMed Central

Gong, Xiaoxing; Shi, Zejin; Wang, Yong; Tian, Yaming; Li, Wenjie; Liu, Lei

2017-01-01

A mature understanding of the sandstone gas reservoir in the Xiaoheba Formation in the southeastern Sichuan Basin remains lacking. To assess the reservoir characteristics and the origin of the high-quality reservoir in the Xiaoheba Formation, this paper uses systematic field investigations, physical property analysis, thin section identification, scanning electron microscopy and electron microprobe methods. The results indicate that the Xiaoheba sandstone is an ultra-tight and ultra-low permeability reservoir, with an average porosity of 2.97% and an average permeability of 0.56×10−3 μm2. This promising reservoir is mainly distributed in the Lengshuixi and Shuangliuba regions and the latter has a relatively high-quality reservoir with an average porosity of 5.28% and average permeability of 0.53×10−3 μm2. The reservoir space comprises secondary intergranular dissolved pores, moldic pores and fractures. Microfacies, feldspar dissolution and fracture connectivity control the quality of this reservoir. The relatively weak compaction and cementation in the interbedded delta front distal bar and interdistributary bay microfacies indirectly protected the primary intergranular pores and enhanced late-stage dissolution. Late-stage potassium feldspar dissolution was controlled by the early-stage organic acid dissolution intensity and the distance from the hydrocarbon generation center. Early-stage fractures acted as pathways for organic acid migration and were therefore important factors in the formation of the reservoir. Based on these observations, the area to the west of the Shuangliuba and Lengshuixi regions has potential for gas exploration. PMID:28686735

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.

Studies of Brazilian meteorites. XIV - Mineralogy, petrology, and chemistry of the Conquista, Minas Gerais, chondrite

NASA Technical Reports Server (NTRS)

Keil, K.; Kirchner, E.; Gomes, C. B.; Jarosewich, E.; Murta, R. L. L.

1978-01-01

The Conquista chondrite is described and classified as an H4. The mineral composition is reported. H-group classification is based on described microscopic, electron microprobe, and bulk chemical studies. The evidence for petrologic type 4 classification includes the pronounced well-developed chondritic texture; the slight compositional variations in constituent phases; the high Ca contents of pyroxene and the presence of pigeonite; glassy to microcrystalline interstitial material rich in alkalis and SiO2; and twinned low-Ca clinopyroxene.

Characterization of crust formation on a parent body of achondrites and the moon by pyroxene crystallography and chemistry

NASA Technical Reports Server (NTRS)

Takeda, H.; Miyamoto, M.; Ishii, T.; Reid, A. M.

1976-01-01

Single crystal X-ray diffraction and electron microprobe techniques were used to study lunar crustal pyroxenes in a cataclastic norite, a pyroxene-rich clast, and anorthosite lunar samples, and also in meteorites including diogenites, eucrites, and the Yamoto (1) howardite. The crystallographic and chemical characteristics of pyroxenes in these materials are compared and are discussed in terms of the lower stability limit of pigeonite. A mechanical mixing model of howardite is proposed.

Experimental verification of the shape of the excitation depth distribution function for AES

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

Tougaard, S.; Jablonski, A.; Institute of Physical Chemistry, Polish Academy of Sciences, ul. Kasprzaka 44/52, 01-224 Warsaw

2011-09-15

In the common formalism of AES, it is assumed that the in-depth distribution of ionizations is uniform. There are experimental indications that this assumption may not be true for certain primary electron energies and solids. The term ''excitation depth distribution function'' (EXDDF) has been introduced to describe the distribution of ionizations at energies used in AES. This function is conceptually equivalent to the Phi-rho-z function of electron microprobe analysis (EPMA). There are, however, experimental difficulties to determine this function in particular for energies below {approx} 10 keV. In the present paper, we investigate the possibility of determining the shape ofmore » the EXDDF from the background of inelastically scattered electrons on the low energy side of the Auger electron features in the electron energy spectra. The experimentally determined EXDDFs are compared with the EXDDFs determined from Monte Carlo simulations of electron trajectories in solids. It is found that this technique is useful for the experimental determination of the EXDDF function.« less

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.

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

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.

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.

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.

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.

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.

Laser Microprobe Mass Spectrometry 1: Basic Principles and Performance Characteristics.

ERIC Educational Resources Information Center

Denoyer, Eric; And Others

1982-01-01

Describes the historical development, performance characteristics (sample requirements, analysis time, ionization characteristics, speciation capabilities, and figures of merit), and applications of laser microprobe mass spectrometry. (JN)

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

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.

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.

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.

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).

SPE-LEEM Studies on the Surface and Electronic Structure of 2-D Transition Metal Dichalcogenides

NASA Astrophysics Data System (ADS)

Yeh, Po-Chun; Jin, Wencan; Zaki, Nader; Zhang, Datong; Sadowski, Jerzy; Al-Mahboob, Abdullah; van de Zande, Arend; Chenet, Daniel; Dadap, Jerry; Herman, Irving; Sutter, Petter; Hone, James; Osgood, Richard

2014-03-01

In this work, we studied the surface and electronic structure of monolayer and few-layer exfoliated MoS2 and WSe2, as well as chemical-vapor-deposition (CVD) grown MoS2, using Spectroscopic Photoemission and Low Energy Electron Microscope (SPE-LEEM). LEEM measurements reveal that, unlike exfoliated MoS2, CVD-grown MoS2 exhibits grain-boundary alterations due to surface strain. However, LEEM and micro-probe low energy electron diffraction show that the quality of CVD-grown MoS2 is comparable to that of exfoliated MoS2. Micrometer-scale angle-resolved photoemission spectroscopy (ARPES) measurement on exfoliated MoS2 and WSe2 single-crystals provides direct evidence for the shifting of the valence band maximum from Γ to K, when the layer number is thinned down to one, as predicted by density functional theory. Our measurements of the k-space resolved electronic structure allow for further comparison with other theoretical predictions and with transport measurements. Session I and II

Electron Microscopy and Analytical X-ray Characterization of Compositional and Nanoscale Structural Changes in Fossil Bone

NASA Astrophysics Data System (ADS)

Boatman, Elizabeth Marie

The nanoscale structure of compact bone contains several features that are direct indicators of bulk tissue mechanical properties. Fossil bone tissues represent unique opportunities to understand the compact bone structure/property relationships from a deep time perspective, offering a possible array of new insights into bone diseases, biomimicry of composite materials, and basic knowledge of bioapatite composition and nanoscale bone structure. To date, most work with fossil bone has employed microscale techniques and has counter-indicated the survival of bioapatite and other nanoscale structural features. The obvious disconnect between the use of microscale techniques and the discernment of nanoscale structure has prompted this work. The goal of this study was to characterize the nanoscale constituents of fossil compact bone by applying a suite of diffraction, microscopy, and spectrometry techniques, representing the highest levels of spatial and energy resolution available today, and capable of complementary structural and compositional characterization from the micro- to the nanoscale. Fossil dinosaur and crocodile long bone specimens, as well as modern ratite and crocodile femurs, were acquired from the UC Museum of Paleontology. Preserved physiological features of significance were documented with scanning electron microscopy back-scattered imaging. Electron microprobe wavelength-dispersive X-ray spectroscopy (WDS) revealed fossil bone compositions enriched in fluorine with a complementary loss of oxygen. X-ray diffraction analyses demonstrated that all specimens were composed of apatite. Transmission electron microscopy (TEM) imaging revealed preserved nanocrystallinity in the fossil bones and electron diffraction studies further identified these nanocrystallites as apatite. Tomographic analyses of nanoscale elements imaged by TEM and small angle X-ray scattering were performed, with the results of each analysis further indicating that nanoscale structure is highly conserved in these four fossil specimens. Finally, the results of this study indicate that bioapatite can be preserved in even the most ancient vertebrate specimens, further supporting the idea that fossilization is a preservational process. This work also underlines the importance of using appropriately selected characterization and analytical techniques for the study of fossil bone, especially from the perspective of spatial resolution and the scale of the bone structural features in question.

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.

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.

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.

Software electron counting for low-dose scanning transmission electron microscopy.

PubMed

Mittelberger, Andreas; Kramberger, Christian; Meyer, Jannik C

2018-05-01

The performance of the detector is of key importance for low-dose imaging in transmission electron microscopy, and counting every single electron can be considered as the ultimate goal. In scanning transmission electron microscopy, low-dose imaging can be realized by very fast scanning, however, this also introduces artifacts and a loss of resolution in the scan direction. We have developed a software approach to correct for artifacts introduced by fast scans, making use of a scintillator and photomultiplier response that extends over several pixels. The parameters for this correction can be directly extracted from the raw image. Finally, the images can be converted into electron counts. This approach enables low-dose imaging in the scanning transmission electron microscope via high scan speeds while retaining the image quality of artifact-free slower scans. Copyright © 2018 The Authors. Published by Elsevier B.V. All rights reserved.

Apollo 15 yellow-brown volcanic glass - Chemistry and petrogenetic relations to green volcanic glass and olivine-normative mare basalts

NASA Technical Reports Server (NTRS)

Hughes, S. S.; Schmitt, R. A.; Delano, J. W.

1988-01-01

Electron microprobe and INAA were used to analyze forty spherules of Apollo 15 yellow-brown glass for major and trace elements. The glass is one of twenty-five high-Mg primary magmas emplaced on the lunar surface in pyroclastic eruptions. The abundances show that the magma was produced by partial melting of differentiated cumulates in the lunar mantle. Models to explain the possible source-regions of several Apollo 15 and Apollo 12 low-Ti mare magmas are presented.

Contamination analyses of technology mirror assembly optical surfaces

NASA Technical Reports Server (NTRS)

Germani, Mark S.

1991-01-01

Automated electron microprobe analyses were performed on tape lift samples from the Technology Mirror Assembly (TMA) optical surfaces. Details of the analyses are given, and the contamination of the mirror surfaces is discussed. Based on the automated analyses of the tape lifts from the TMA surfaces and the control blank, we can conclude that the particles identified on the actual samples were not a result of contamination due to the handling or sampling process itself and that the particles reflect the actual contamination on the surface of the mirror.

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.

Studies related to the surfaces of the moon and planets. [a discussion of vapor deposition and glasses of lunar composition

NASA Technical Reports Server (NTRS)

Hapke, B.

1974-01-01

A variety of glasses of lunar composition were prepared with different amounts of Fe and Ti under both reducing and oxidizing conditions, and also by sputter-deposition and thermal evaporation and condensation. These materials were analyzed by wet chemical, electron microprobe, ESR, Mossbauer and magnetic methods. The effects of darkening processes on surface soils of airless bodies are discussed along with the effects of vapor phase deposition processes on the optical, chemical, and magnetic properties of the lunar regolith.

As-received microstructure of a SiC/Ti-15-3 composite

NASA Technical Reports Server (NTRS)

Lerch, Bradley A.; Hull, David R.; Leonhardt, Todd A.

1988-01-01

A silicon carbide fiber reinforced titanium (Ti-15V-3Cr-3Sn-3Al) composite is metallographically examined. Several methods for examining composite materials are investigated and documented. Polishing techniques for this material are described. An interference layering method is developed to reveal the structure of the fiber, the reaction zone, and various phases within the matrix. Microprobe and transmission electron microscope (TEM) analyses are performed on the fiber/matrix interface. A detailed description of the fiber distribution as well as the microstructure of the fiber and matrix are presented.

Evaluation of hot corrosion behavior of thermal barrier coatings

NASA Technical Reports Server (NTRS)

Hodge, P. E.; Miller, R. A.; Gedwill, M. A.

1980-01-01

Calcium silicate and yttria stabilized zirconia/MCrAlY thermal barrier coating systems on air-cooled specimens were exposed to sodium plus vanadium doped Mach 0.3 combustion gases. Thermal barrier coating endurance was determined to be a strong inverse function of ceramic coating thickness. Coating system durability was increased through the use of higher Cr + Al NiCrAl and CoCrAlY bond coatings. Chemical and electron microprobe analyses supported the predictions of condensate compositions and the determination of their roles in causing spalling of the ceramic coatings.

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.)

Coexisting cummingtonite and aluminous hornblende from garnet amphibolite, Boehls Butte area, Idaho, USA

USGS Publications Warehouse

Hietanen, A.

1973-01-01

Electron microprobe analyses of green hornblende and coexisting cummingtonite from garnet amphibolite show identical Fe/Mg ratios ( = 0.9). Cummingtonite is iron-magnesium silicate with very little calcium and aluminum and practically no alkalies. In contrast, the hornblende has 1.5 tetrahedral Al, 0.9 octahedral Al and a considerable amount of Ca and alkalies. Comparison with the hornblendes from the Sierra Nevada shows a higher relative amount of tschemakite molecule in the hornblendes from Idaho where pressures during the recrystallization were higher. ?? 1973.

Zircon crystal morphology and internal structures as a tool for constraining magma sources: Examples from northern Portugal Variscan biotite-rich granite plutons

NASA Astrophysics Data System (ADS)

Brites Martins, Helena C.; Simões, Pedro P.; Abreu, Joana

2014-09-01

In northern Portugal, large volumes of granitoids were emplaced during the last stage (D3) of the Variscan orogeny and display a wide range of petrological signatures. We studied the morphologies and internal structures of zircons from syn-, late- and post-D3 granitoids. The sin-D3 granitoids include the Ucanha-Vilar, Lamego, Felgueiras, Sameiro, and Refoios do Lima plutons, the late- and post-D3 granitoids are represented by the Vieira do Minho and the Vila Pouca de Aguiar plutons, respectively. Typological investigations after Pupin (1980) along with scanning electron microprobe imaging reveal that the external morphology of zircon changes consistently with a decrease in the crystallization temperature. Zircon populations from the Refoios do Lima and the Vieira do Minho granites show gradual changes in the internal morphologies and their typologic evolution trends are consistent with their mainly crustal origin. The Sameiro, Felgueiras, Lamego and Ucanha-Vilar granites have more complex internal and external morphology and typological evolution trends that cross the domain of the calc-alkaline to the aluminous granites compatible with a mixing process. Finally, the morphological types of the Vila Pouca de Aguiar granites are found both in calc-alkaline and sub-alkaline granites and their typological evolutionary trends follow the calc-alkaline/sub-alkaline trend, suggesting crustal sources with some mantle contribution.

Crack Coalescence in Molded Gypsum and Carrara Marble

NASA Astrophysics Data System (ADS)

Wong, N.; Einstein, H. H.

2007-12-01

This research investigates the fracturing and coalescence behavior in prismatic laboratory-molded gypsum and Carrara marble specimens, which consist of either one or two pre-existing open flaws, under uniaxial compression. The tests are monitored by a high speed video system with a frame rate up to 24,000 frames/second. It allows one to precisely observe the cracking mechanisms, in particular if shear or tensile fracturing takes place. Seven crack types and nine crack coalescence categories are identified. The flaw inclination angle, the ligament length and the bridging angle between two flaws have different extents of influence on the coalescence patterns. For coplanar flaws, as the flaw inclination angle increases, there is a general trend of variation from shear coalescence to tensile coalescence. For stepped flaws, as the bridging angle changes from negative to small positive, and further up to large positive values, the coalescence generally progresses from categories of no coalescence, indirect coalescence to direct coalescence. For direct coalescence, it generally progresses from shear, mixed shear-tensile to tensile as the bridging angle increases. Some differences in fracturing and coalescence processes are observed in gypsum and marble, particularly the crack initiation in marble is preceded by the development of macroscopic white patches, but not in gypsum. Scanning Electron Microprobe (SEM) study reveals that the white patches consist of zones of microcracks (process zones).

Slickenside formation by surface melting during the mechanical excavation of rock

NASA Astrophysics Data System (ADS)

Spray, John G.

This work discusses the nature and origin of slickensides generated by the impingement of high-carbon steel teeth on sandstone during the mechanical excavation of boulders by back shovel and front loader. The slickensides show a number of morphological features that can be related to the direction and sense of tooth displacement, including striations, carrot-shaped grooves, curved fractures and steps. Scanning and transmission electron microscopy reveal that the slickensides comprise a layer of Fe-enriched, glass-bonded gouge (≤150 μm thick). The estimated shear stresses and velocities realized at the tooth-rock interface (175 MPa at 1 m s -1 for the back shovel and 100 MPa at 2 m s -1 for the front loader) indicate that a heat production of 150-200 MW m -2 and mean surface temperature of 1400-1700°C were achieved. XRF and microprobe analyses confirm that localized bulk melting and Fe-enrichment of the surface occurred during slip. The excavator-generated slickensides provide an analogue for the effects of a single co-seismic event in the evolution of a shallow, relatively dry fault surface. From a simple consideration of energetics under these conditions, it is apparent that localized surface melting should be commonplace. Such an analogue may be useful as a guide for recognizing melt features in natural slickensides, features that would otherwise tend to be obscured during lengthier periods of interseismic surface modification.

Thermodynamics of arsenates, selenites and sulfates in the oxidation zone of sulfide ores: XII. Mineral equilibria in the Cd-Se-H2O system at 25°C

NASA Astrophysics Data System (ADS)

Charykova, M. V.; Vishnevsky, A. V.; Krivovichev, V. G.; Fokina, E. L.; Ivanova, N. M.; Platonova, N. V.; Semenova, V. V.

2016-12-01

Understanding the mechanisms of cadmium and selenium behavior under near-surface conditions is very important for solving certain environmental problems. The principal aim of this study is physicochemical analysis of the formation conditions of synthetic cadmium selenite CdSeO3 · H2O and experimental investigation of its thermal stability and dehydration and dissociation mechanisms. The synthesis was performed by boiling-dry aqueous solutions of cadmium nitrate and sodium selenite. The obtained samples were identified with electron microprobe and powder X-ray diffraction. Complex thermal analysis (thermogravimetry and differential scanning calorimetry) have shown that CdSeO3 · H2O is dehydrated at 177-241°C in two stages, apparently corresponding to the formation of CdSeO3 · 2/3H2O. The Eh-pH diagrams were calculated using the Geochemist's Workbench (GWB 9.0) software package. The Eh-pH diagrams have been calculated for the Cd-Se-H2O and Cd-Se-CO2-H2O systems for the average content of these elements in underground waters. The formation of cadmium selenite, CdSeO3 · H2O in the oxidation medium is quite possible. The existence of CdSeO3 is possible at high temperature.

Si Isotopes of Brownleeite

NASA Technical Reports Server (NTRS)

Nakamura-Messenger, K.; Messenger, Scott R.; Ito, M.; Keller, L. P.; Clemett, S. J.; Jones, J. H.; Tatsuoka, H.; Zolensky, M. E.; Tatsuoka, H.

2010-01-01

Brownleeite is a manganese silicide, ideally stoichiometric MnSi, not previously observed in nature until its discovery within an interplanetary dust particle (IDP) that likely originated from a comet [1]. Three discrete brownleeite grains in the IDP L2055 I3 (4 microns in size, hereafter IDP I3) were identified with maximum dimensions of 100, 250 and 600 nm and fully analyzed using scanning-transmission electron microscopy (STEM) [1]. One of the grains (100 nm in size) was poikilitically enclosed by low-Fe, Mn-enriched (LIME) olivine. LIME olivine is epitaxial to the brownleeite with the brownleeite (200) parallel to the olivine c* [1]. LIME olivine is an enigmatic phase first reported from chondritic porous IDPs and some unequilibrated ordinary chondrites [ 2], that is commonly observed in chondritic-porous IDPs. Recently, LIME olivine has been also found in comet Wild-2 (Stardust) samples [3], indicating that LIME olivine is a common mineral component of comets. LIME olivine has been proposed to form as a high temperature condensate in the protosolar nebula [2]. Brownleeite grains also likely formed as high-temperature condensates either in the early Solar System or in the outflow of an evolved star or supernova explosion [1]. The isotopic composition of the brownleeite grains may strongly constrain their ultimate source. To test this hypothesis, we performed isotopic analyses of the brownleeite and the associated LIME olivine, using the NASA/JSC NanoSIMS 50L ion microprobe.

Mineralogical Studies Related to Endemic Diseases in Rural P. R. China

NASA Astrophysics Data System (ADS)

Belkin, H. E.; Zheng, B.; Finkelman, R. B.

2003-12-01

Domestic combustion of coal for heating and cooking is mostly confined to the world's developing countries and probably involves about 1 billion persons in China, India, Indonesia, and Africa. Various endemic diseases affecting millions of people involving arsenic, selenium, and fluorine poisoning have been associated with domestic coal combustion in rural China. We have investigated the relationship between mineralized coals (and stone coals) and disease occurrences in Guizhou and Hubei Provinces. The mineralogy of the coals has been studied by a wide variety of techniques, including optical petrography, scanning electron microscopy, electron microprobe analysis, ion probe, Synchrotron XANES-EXAFS, and Raman spectroscopy. Arsenic enrichment (up to 3 weight percent) in Upper Permian Longtan Formation coals, southwestern Guizhou Province, occurs in both 3+ and 5+ valence states. Arsenic occurs in arsenopyrite, pyrite, Al-phosphate, scorodite, Fe-oxides, and as an organically-bound species. Fluorine poisoning, much more widespread than arsenic-poisoning, is related to burning F-rich coals and F-rich clays as admixtures. Mineralogical and chemical analysis suggests that the clays contain the fluorine probably substituting for the hydroxyl group. Localized selenium poisoning in Hubei Province is related to Se-rich stone coals. The selenium occurs as a native element and in rare mandarinoite. In these three cases, knowledge of the paragenesis and mineralogy of the element enrichment in coal was vital to help understand and mitigate the endemic diseases. For the situation concerning arsenic and selenium poisoning, suspect coals have been identified and mining from these deposits has been curtailed. Fluorine has been a much more difficult problem for the local public health officials as both the coal and clay in the burning admixture can contain high fluorine. Regional geochemical and mineralogical studies will help to define coal and clay with low fluorine, suitable for domestic use.

Reverse Engineering of Corinthian Pigment Processing and Firing Technologies on Archaic Polychrome Ceramics

NASA Astrophysics Data System (ADS)

Klesner, Catherine Elizabeth

Decorative, polychrome ceramics from Corinth, Greece, produced during the 8th-6th centuries B.C.E. are luxury goods that were widely traded throughout Greece and the Mediterranean. The decorated ceramics were produced in a variety of shapes, including aryballos, alabastron, and olpe. They were decorated with slip-glazes in distinctive white, black, red, yellow, and purple colors, and in a variety of surface finishes, matte, semi-matte and glossy. Artisans in Corinthian workshops experimented to change the colors of the slips by varying the type and amount of iron-rich raw materials. They also varied the composition of the clay used as a binder and the amount of flux used as a sintering aid to promote glass formation. This research reconstructs the technology used by the Corinthian craftsmen to produce the Archaic polychrome ceramics, and shows how these technologies differed from the production of better known, more prestigious Athenian black-figure and red-figure ceramics. Through microstructural examination of archaeological samples and replication experiments, this thesis proposes that the purple iron oxide pigment is the result of acid treatment and oxidation of iron metal. The firing temperature range of the Corinthian polychrome ceramics was determined experimentally to be 925-1025°C, which is higher than previously reported and similar to that reported for Corinthian transport amphoras. The firing range is higher by 50-150°C than the Athenian black-figure and red-figure ceramics. Samples of Corinthian polychrome and Athenian black-figure ceramics from the Marie Farnsworth collection at the University of Arizona were tested and compared to Corinthian clay collections. Analytical techniques included Fourier-transform infrared spectroscopy (FTIR), scanning-electron microscopy with energy-dispersive spectroscopy (SEM-EDS), micro-Raman spectroscopy, and wavelength-dispersive electron microprobe (EPMA with BSE-SEM).

The 2003 phreatomagmatic eruptions of Anatahan volcano - Textural and petrologic features of deposits at an emergent island volcano

USGS Publications Warehouse

Pallister, J.S.; Trusdell, F.A.; Brownfield, I.K.; Siems, D.F.; Budahn, J.R.; Sutley, S.F.

2005-01-01

Stratigraphic and field data are used in conjunction with textural and chemical evidence (including data from scanning electron microscope, electron microprobe, X-ray fluorescence, X-ray diffraction, and instrumental neutron activation analysis) to establish that the 2003 eruption of Anatahan volcano was mainly phreatomagmatic, dominated by explosive interaction of homogeneous composition low-viscosity crystal-poor andesite magma with water. The hydromagmatic mode of eruption contributed to the significant height of initial eruptive columns and to the excavation and eruption of altered rock debris from the sub-volcanic hydrothermal system. Volatile contents of glass inclusions in equilibrium phenocrysts less abundances of these constituents in matrix glass times the estimated mass of juvenile magma indicate minimum emissions of 19 kt SO2 and 13 kt Cl. This petrologic estimate of SO2 emission is an order-of-magnitude less than an estimate from TOMS. Similarly, inferred magma volumes from the petrologic data are an order of magnitude greater than those modeled from deformation data. Both discrepancies indicate additional sources of volatiles, likely derived from a separate fluid phase in the magma. The paucity of near-source volcanic-tectonic earthquakes preceding the eruption, and the dominance of sustained long-period tremor are attributed to the ease of ascent of the hot low-viscosity andesite, followed by a shallow phreatomagmatic mode of eruption. Phreatomagmatic eruptions are probably more common at emergent tropical island volcanoes, where shallow fresh-water lenses occur at near-sea-level vents. These relations suggest that phreatomagmatic explosions contributed to the formation of many of the near-sea-level craters and possibly even to the small calderas at the other Mariana islands.

Melting of Fe-Si-O alloys: the Fate of Coexisting Si and O in the Core

NASA Astrophysics Data System (ADS)

Arveson, S. M.; Lee, K. K. M.

2017-12-01

The light element budget of Earth's core plays an integral role in sustaining outer core convection, which powers the geodynamo. Many experiments have been performed on binary iron compounds, but the results do not robustly agree with seismological observations and geochemical constraints. Earth's core is almost certainly made up of multiple light elements, so the future of core composition studies lies in ternary (or higher order) systems in order to examine interactions between light elements. We perform melting experiments on Fe-Si-O alloys in a laser-heated diamond-anvil cell to 80 GPa and 4000 K. Using 2D multi- wavelength imaging radiometry together with textural and chemical analysis of quenched samples, we measure the high-pressure melting curves and determine partitioning of light elements between the melt and the coexisting solid. Quenched samples are analyzed both in map view and in cross section using scanning electron microscopy (SEM) and electron microprobe analysis (EPMA) to examine the 3D melt structure and composition. Partitioning of light elements between molten and solid alloys dictates (1) the density contrast at the ICB, which drives compositional convection in the outer core and (2) the temperature of the CMB, an integral parameter for understanding the deep Earth. Our experiments suggest silicon and oxygen do not simply coexist in the melt and instead show complex solubility based on temperature. Additionally, we do not find evidence of crystallization of SiO2 at low oxygen content as was recently reported.11 Hirose, K., et al., Crystallization of silicon dioxide and compositional evolution of the Earth's core. Nature, 2017. 543(7643): p. 99-102.

Arsenic-bearing pyrite and marcasite in the Fire Clay coal bed, Middle Pennsylvanian Breathitt Formation, eastern Kentucky

USGS Publications Warehouse

Ruppert, L.F.; Hower, J.C.; Eble, C.F.

2005-01-01

Arsenic concentrations determined on 11 lithotype samples from the Middle Pennsylvanian Breathitt Group Fire Clay coal bed, Leslie County, KY, range from 1 to 418 ppm (whole coal basis). The 11 lithotype samples, which vary in thickness from 4 to 18 cm, were sampled from a continuous 1.38 m channel sample, and were selected based on megascopic appearance (vitrain-rich versus attrital-rich). A lithotype that contains 418 ppm As is located near the top of the coal bed and is composed of 10.5 cm of bright clarain bands containing fusain that, within short distances, grade laterally into Fe sulfide bands. To determine the mode of occurrence of As in this lithotype, the coal was examined with scanning electron microscopy and analyzed by energy dispersive X-ray fluorescence. Massive, framboidal, cell filling, cell-wall replacement, and radiating forms of Fe sulfide were observed in the high As lithotype; many of the radiating Fe sulfide forms, and one of the cell-wall replacements contained As. Examination of the grains with optical light microscopy shows that the majority of radiating morphologies are pyrite, the remainder are marcasite. Selected Fe sulfide grains were also analyzed by electron microprobe microscopy. Arsenic concentrations within individual grains range from 0.0 wt.% to approximately 3.5 wt.%. On the basis of morphology, these Fe sulfides are presumed to be of syngenetic origin and would probably be removed from the coal during physical coal cleaning, thus eliminating a potential source of As from the coal combustion process. However, because the grains are radiating and have high surface area, dissolution and release of As could occur if the pyrite is oxidized in refuse ponds.

Multi-scale analysis of the occurrence of Pb, Cr and Mn in the NIST standards: Urban dust (SRM 1649a) and indoor dust (SRM 2584)

NASA Astrophysics Data System (ADS)

Jiang, Mingyu; Nakamatsu, Yuki; Jensen, Keld A.; Utsunomiya, Satoshi

2014-01-01

Adverse health effects of ambient particulate matters are closely related to the speciation of the constituting organic matters and toxic metals. To determine multi-parameters of the metal speciation in urban and indoor dusts, we have performed systematic bulk- to nano-scale (“multi-scale”) analysis on the speciation of Pb, Mn, and Cr in two National Institute of Standards and Technology (NIST) standard reference materials (SRMs): urban dust (SRM 1649a) and indoor dust (SRM 2584), utilizing X-ray absorption near-edge structure, powder X-ray diffraction analysis, electron microprobe analysis, scanning electron microscopy, and transmission electron microscopy. Major crystalline phases are quartz, gypsum, kaolinite, and muscovite in SRM 1649a, while quartz, gypsum, calcite, and possibly muscovite (or chabazite) in SRM 2584. A number of Pb sulfate nanoparticles (50-200 nm) occur in SRM 1649a, whereas micron-sized Pb carbonate is present containing various concentrations of Zn and Ti in the complex texture in SRM 2584. Relatively soluble Mn(II) sulfate is the bulk-averaged Mn speciation in SRM 1649a, although discrete Mn sulfate particles are not characterized by individual particle analysis, implying the diluted Mn distribution within other sulfate. In SRM 2584, Mn speciation includes a mixture of oxides and carbonates, and trace Mn in chromite. Chromite (FeCr2O4) is the major Cr speciation in SRM1694a, while unidentified Cr(III) phases with minor chromite and Pb chromate are present in SRM 2584, among which the Pb chromate is composed of Cr(VI). A significant number of the metal-bearing particles are distributed to the submicron-size fraction in the urban dust, SRM 1649a, suggesting that these metal nanoparticles can potentially penetrate into the deep respiratory system. This study demonstrates that multi-scale analysis combining nano and bulk analytical techniques is a powerful approach to investigate the multi-parameters of metal-bearing nanoparticles in heterogeneous PM samples.

Characterization of Meteorites by Focused Ion Beam Sectioning: Recent Applications to CAIs and Primitive Meteorite Matrices

NASA Technical Reports Server (NTRS)

Christoffersen, Roy; Keller, Lindsay P.; Han, Jangmi; Rahman, Zia; Berger, Eve L.

2015-01-01

Focused ion beam (FIB) sectioning has revolutionized preparation of meteorite samples for characterization by analytical transmission electron microscopy (TEM) and other techniques. Although FIB is not "non-destructive" in the purest sense, each extracted section amounts to no more than nanograms (approximately 500 cubic microns) removed intact from locations precisely controlled by SEM imaging and analysis. Physical alteration of surrounding material by ion damage, fracture or sputter contamination effects is localized to within a few micrometers around the lift-out point. This leaves adjacent material intact for coordinate geochemical analysis by SIMS, microdrill extraction/TIMS and other techniques. After lift out, FIB sections can be quantitatively analyzed by electron microprobe prior to final thinning, synchrotron x-ray techniques, and by the full range of state-of-the-art analytical field-emission scanning transmission electron microscope (FE-STEM) techniques once thinning is complete. Multiple meteorite studies supported by FIB/FE-STEM are currently underway at NASA-JSC, including coordinated analysis of refractory phase assemblages in CAIs and fine-grained matrices in carbonaceous chondrites. FIB sectioning of CAIs has uncovered epitaxial and other overgrowth relations between corundum-hibonite-spinel consistent with hibonite preceding corundum and/or spinel in non-equilibrium condensation sequences at combinations of higher gas pressures, dust-gas enrichments or significant nebular transport. For all of these cases, the ability of FIB to allow for coordination with spatially-associated isotopic data by SIMS provides immense value for constraining the formation scenarios of the particular CAI assemblage. For carbonaceous chondrites matrix material, FIB has allowed us to obtain intact continuous sections of the immediate outer surface of Murchison (CM2) after it has been experimentally ion processed to simulate solar wind space weathering. The surface amorphization and loss of OH produced by the irradiation provides important clues regarding space weathering on primitive asteroids such as the OSIRIS-Rex target 101955 Bennu.

Near infrared spectra of muscovite, Tschermak substitution, and metamorphic reaction progress: Implications for remote sensing

NASA Astrophysics Data System (ADS)

Duke, Edward F.

1994-07-01

Near infrared (NIR) spectra of Precambrian metagraywacke in the Black Hills, South Dakota, demonstrate that reflectance spectroscopy can be used to monitor progressive changes in mineral chemistry as a function of metamorphic grade. The wavelength of a combination Al-O-H absorption band in muscovite, measured using both laboratory and field-portable NIR spectrometers, shifts from 2217 nm in the biotite zone to 2199 nm in the sillimanite + K-feldspar zone. The band shift corresponds to an increase in the Alvi content of muscovite, determined by electron microprobe, and is thus a monitor of Al2Si-1(Fe,Mg)-1 (Tschermak) exchange. Spectroscopic measurements such as these are useful in the case of aluminum-deficient rocks, which lack metamorphic index minerals or appropriate assemblages for thermobarometric studies, and in low-grade rocks (subgarnet zone), which lack quantitative indicators of metamorphic grade and are too fine grained for petrographic or microprobe studies. More important, spectroscopic detection of mineral-chemical variations in metamorphic rocks provides petrologists with a tool to recover information on metamorphic reaction histories from high-spectral-resolution aircraft or satellite remote sensing data.

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.

Diagenetic variation at the lamina scale in lacustrine organic-rich shales: Implications for hydrocarbon migration and accumulation

NASA Astrophysics Data System (ADS)

Liang, Chao; Cao, Yingchang; Liu, Keyu; Jiang, Zaixing; Wu, Jing; Hao, Fang

2018-05-01

Lacustrine carbonate-rich shales are well developed within the Mesozoic-Cenozoic strata of the Bohai Bay Basin (BBB) of eastern China and across southeast Asia. Developing an understanding of the diagenesis of these shales is essential to research on mass balance, diagenetic fluid transport and exchange, and organic-inorganic interactions in black shales. This study investigates the origin and distribution of authigenic minerals and their diagenetic characteristics, processes, and pathways at the scale of lacustrine laminae within the Es4s-Es3x shale sequence of the BBB. The research presented in this study is based on thin sections, field emission scanning electron microscope (FESEM) and SEM-catholuminescence (CL) observations of well core samples combined with the use of X-ray diffraction (XRD), energy dispersive spectroscopy, electron microprobe analysis, and carbon and oxygen isotope analyses performed using a laser microprobe mass spectrometer. The dominant lithofacies within the Es4s-Es3x sequence are a laminated calcareous shale (LCS-1) and a laminated clay shale (LCS-2). The results of this study show that calcite recrystallization1 is the overarching diagenetic process affecting the LCS-1, related to acid generation from organic matter (OM) thermal evolution. This evolutionary transition is the key factor driving the diagenesis of this lithofacies, while the transformation of clay minerals is the main diagenetic attribute of the LCS-2. Diagenetic differences occur within different laminae and at variable locations within the same lamina level, controlled by variations in mineral composition and the properties of laminae interfaces. The diagenetic fluid migration scale is vertical and responses (dissolution and replacement) are limited to individual laminae, between zero and 100 μm in width. In contrast, the dominant migration pathway for diagenetic fluid is lateral, along the abrupt interfaces between laminae boundaries, which leads to the vertical transmission of diagenetic responses. The recrystallization boundaries between calcite laminae act as the main migration pathways for the expulsion of hydrocarbons from these carbonate-rich lacustrine shales. However, because the interaction between diagenetic fluids and the shales themselves is limited to the scale of individual lamina, this system is normally closed. The occurrence of abnormal pressure fractures can open the diagenetic system, however, and cause interactions to occur throughout laminae; in particular, the closed-open (C-O) diagenetic process at this scale is critical to this shale interval. Multi-scale C-O systems are ubiquitous and episodic ranging from the scale of laminae to the whole basin. Observations show that such small-scale systems are often superimposed onto larger ones to constitute the complex diagenetic system seen within the BBB combining fluid transport, material and energy exchange, and solid-liquid and organic-inorganic interactions.

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.

Moessbauer and Electron Microprobe Studies of Density Separates of Martian Nakhlite Mil03346: Implications for Interpretation of Moessbauer Spectra Acquired by the Mars Exploration Rovers

NASA Technical Reports Server (NTRS)

Morris, R. V.; McKay, G. A.; Agresti, D. G.; Li, Loan

2008-01-01

Martian meteorite MIL03346 is described as an augite-rich cumulate rock with approx.80%, approx.3%, and approx.21% modal phase proportions of augite (CPX), olivine and glassy mesostasis, respectively, and is classified as a nakhlite [1]. The Mossbauer spectrum for whole rock (WR) MIL 03346 is unusual for Martian meteorites in that it has a distinct magnetite subspectrum (7% subspectral area) [2]. The meteorite also has products of pre-terrestrial aqueous alteration ("iddingsite") that is associated primarily with the basaltic glass and olivine. The Mossbauer spectrometers on the Mars Exploration Rovers have measured the Fe oxidation state and the Fe mineralogical composition of rocks and soils on the planet s surface since their landing in Gusev Crater and Meridiani Planum in January, 2004 [3,4]. The MIL 03346 meteorite provides an opportunity to "ground truth" or refine Fe phase identifications. This is particularly the case for the so-called "nanophase ferric oxide" (npOx) component. NpOx is a generic name for a ferric rich product of oxidative alteration. On Earth, where we can take samples apart and study individual phases, examples of npOx include ferrihydrite, schwertmannite, akagaaneite, and superparamagnetic (small particle) goethite and hematite. It is also possible for ferric iron to be associated to some unknown extent with igneous phases like pyroxene. We report here an electron microprobe (EMPA) and Moessbauer (MB) study of density separates of MIL 03346. The same separates were used for isotopic studies by [5]. Experimental techniques are described by [6,7].

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.

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

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.

Optimisation d'analyses de grenat almandin realisees au microscope electronique a balayage

NASA Astrophysics Data System (ADS)

Larose, Miguel

The electron microprobe (EMP) is considered as the golden standard for the collection of precise and representative chemical composition of minerals in rocks, but data of similar quality should be obtainable with a scanning electron microscope (SEM). This thesis presents an analytical protocol aimed at optimizing operational parameters of an SEM paired with an EDS Si(Li) X-ray detector (JEOL JSM-840A) for the imaging, quantitative chemical analysis and compositional X-ray maps of almandine garnet found in pelitic schists from the Canadian Cordillera. Results are then compared to those obtained for the same samples on a JEOL JXA 8900 EMP. For imaging purposes, the secondary electrons and backscattered electrons signals have been used to obtain topographic and chemical contrast of the samples, respectively. The SEM allows the acquisition of images with higher resolution than the EMP when working at high magnifications. However, for millimetric size minerals requiring very low magnifications, the EMP can usually match the imaging capabilities of an SEM. When optimizing images for both signals, the optimal operational parameters to show similar contrasts are not restricted to a unique combination of values. Optimization of operational parameters for quantitative chemical analysis resulted in analytical data with a similar precision and showing good correlation to that obtained with an EMP. Optimization of operational parameters for compositional X-ray maps aimed at maximizing the collected intensity within a pixel as well as complying with the spatial resolution criterion in order to obtain a qualitative compositional map representative of the chemical variation within the grain. Even though various corrections were needed, such as the shadow effect and the background noise removal, as well as the impossibility to meet the spatial resolution criterion because of the limited pixel density available on the SEM, the compositional X-ray maps show a good correlation with those obtained with the EMP, even for concentrations as low as 0,5%. When paired with a rigorous analytical protocol, the use of an SEM equipped with an EDS Si (Li) X-ray detector allows the collection of qualitative and quantitative results similar to those obtained with an EMP for all three of the applications considered.

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.

System and method for compressive scanning electron microscopy

DOEpatents

Reed, Bryan W

2015-01-13

A scanning transmission electron microscopy (STEM) system is disclosed. The system may make use of an electron beam scanning system configured to generate a plurality of electron beam scans over substantially an entire sample, with each scan varying in electron-illumination intensity over a course of the scan. A signal acquisition system may be used for obtaining at least one of an image, a diffraction pattern, or a spectrum from the scans, the image, diffraction pattern, or spectrum representing only information from at least one of a select subplurality or linear combination of all pixel locations comprising the image. A dataset may be produced from the information. A subsystem may be used for mathematically analyzing the dataset to predict actual information that would have been produced by each pixel location of the image.

Stardust Interstellar Preliminary Examination

NASA Astrophysics Data System (ADS)

Westphal, A.; Stardust Interstellar Preliminary Examation Team: http://www. ssl. berkeley. edu/~westphal/ISPE/

2011-12-01

A. J. Westphal, C. Allen, A. Ansari, S. Bajt, R. S. Bastien, H. A. Bechtel, J. Borg, F. E. Brenker, J. Bridges, D. E. Brownlee, M. Burchell, M. Burghammer, A. L. Butterworth, A. M. Davis, P. Cloetens, C. Floss, G. Flynn, D. Frank, Z. Gainsforth, E. Grün, P. R. Heck, J. K. Hillier, P. Hoppe, G. Huss, J. Huth, B. Hvide, A. Kearsley, A. J. King, B. Lai, J. Leitner, L. Lemelle, H. Leroux, R. Lettieri, W. Marchant, L. R. Nittler, R. Ogliore, F. Postberg, M. C. Price, S. A. Sandford, J.-A. Sans Tresseras, T. Schoonjans, S. Schmitz, G. Silversmit, A. Simionovici, V. A. Solé, R. Srama, T. Stephan, V. Sterken, J. Stodolna, R. M. Stroud, S. Sutton, M. Trieloff, P. Tsou, A. Tsuchiyama, T. Tyliszczak, B. Vekemans, L. Vincze, D. Zevin, M. E. Zolensky, >29,000 Stardust@home dusters ISPE author affiliations are at http://www.ssl.berkeley.edu/~westphal/ISPE/. In 2000 and 2002, a ~0.1m2 array of aerogel tiles and alumi-num foils onboard the Stardust spacecraft was exposed to the interstellar dust (ISD) stream for an integrated time of 200 days. The exposure took place in interplanetary space, beyond the orbit of Mars, and thus was free of the ubiquitous orbital debris in low-earth orbit that precludes effective searches for interstellar dust there. Despite the long exposure of the Stardust collector, <<100 ISD particles are expected to have been captured. The particles are thought to be ~1μm or less in size, and the total ISD collection is probably <10-6 by mass of the collection of cometary dust parti-cles captured in the Stardust cometary dust collector from the coma of the Jupiter-family comet Wild 2. Thus, although the first solid sample from the local interstellar medium is clearly of high interest, the diminutive size of the particles and the low numbers of particles present daunting challenges. Nevertheless, six recent developments have made a Preliminary Examination (PE) of this sample practical: (1) rapid automated digital optical scanning microscopy for three-dimensional imaging of the aerogel collector; (2) rapid automated digital scanning electron microscopy for imaging of the aluminum foils; (3) an effective, massively-distributed search by citizen scientists through the Internet; (4) extraction and sample preparation tech-niques for μm-sized particles in aerogel; (5) advances in capabili-ties of synchrotron infrared and X-ray microprobes that enable non-destructive analyses of sub-μm particles in situ in aerogel; and (6) the development of focused-ion beam (FIB) milling tech-niques for sample preparation. The Stardust Interstellar PE consists of six related projects: the identification of tracks through automated scanning microscopy and distributed searching by volunteers (Stardust@home); the extraction of tracks from aerogel in "picokeystones"; the analysis of tracks using synchrotron microprobes; the identifica-tion and analysis of impacts in aluminum foils; laboratory investigations of ISD analogs using an electrostatic dust accelerator; and modeling of ISD propagation in the heliosphere. To date we have identified four impacts in the aerogel collector and one on the foils of probable interstellar origin. We will report on our analyses and implications for the solid component of the local interstellar medium.

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

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.

Sulfur speciation in hydrous experimental glasses of varying oxidation state - Results from measured wavelength shifts of sulfur X-rays

NASA Technical Reports Server (NTRS)

Carroll, Michael R.; Rutherford, Malcolm J.

1988-01-01

The focusing geometry of an electron microprobe has been used to measure the wavelength shifts of sulfur X-rays from hydrous experimental melts synthesized at oxygen fugacities that range from near the iron-wustite buffer to the magnetite-hermatite buffer. It is found that the proportion of dissolved sulfur which is present as sulfate increases with increasing oxygen fugacity. It is noted that in natural melts that have equilibrated at or below fayalite-magnetite-quartz values of +1, sulfur is probably present mainly as S(2-).

JSC Mars-1 Martian Soil Simulant: Melting Experiments and Electron Microprobe Studies

NASA Technical Reports Server (NTRS)

Carpenter, P.; Sebille, L.; Boles, W.; Chadwell, M.; Schwarz, L.

2003-01-01

JSC Mars-1 has been developed as a Martian regolith simulant, and is the <1 mm size fraction of a palagonitic tephra (a glassy volcanic ash altered at low temperatures) from Pu'u Nene cinder cone on the Island of Hawaii. The Mars-1 simulant forms the basis for numerous terrestrial studies which aim to evaluate the suitability of Martian soil for materials processing. Martian soil may be sintered to form building materials for construction, and also melted or reacted to extract metals for various uses, as well as oxygen for life support.

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.

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.

Annealing effects in plated-wire memory elements. I - Interdiffusion of copper and Permalloy.

NASA Technical Reports Server (NTRS)

Knudson, C. I.; Kench, J. R.

1971-01-01

Results of investigations using X-ray diffraction and electron-beam microprobe techniques have shown that copper and Permalloy platings interdiffuse at low temperatures when plated-wire memory elements are annealed for times as short as 50 hr. Measurable interdiffusion between Permalloy platings and gold substrates does not occur in similar conditions. Both magnetic and compositional changes during aging are found to occur by a thermally activated process with activation energies around 38 kcal/mol. It is shown, however, that copper-diffusion and magnetic-dispersion changes during aging are merely concurrent processes, neither being the other's cause.

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.

Synchronized voltage contrast display analysis system

NASA Technical Reports Server (NTRS)

Johnston, M. F.; Shumka, A.; Miller, E.; Evans, K. C. (Inventor)

1982-01-01

An apparatus and method for comparing internal voltage potentials of first and second operating electronic components such as large scale integrated circuits (LSI's) in which voltage differentials are visually identified via an appropriate display means are described. More particularly, in a first embodiment of the invention a first and second scanning electron microscope (SEM) are configured to scan a first and second operating electronic component respectively. The scan pattern of the second SEM is synchronized to that of the first SEM so that both simultaneously scan corresponding portions of the two operating electronic components. Video signals from each SEM corresponding to secondary electron signals generated as a result of a primary electron beam intersecting each operating electronic component in accordance with a predetermined scan pattern are provided to a video mixer and color encoder.

Swept Line Electron Beam Annealing of Ion Implanted Semiconductors.

DTIC Science & Technology

1982-07-01

of my research to the mainstream of technology. The techniques used for beam processing are distinguished by their * ~.* beam source and method by...raster scanned CW lasers (CWL), pulsed ion beams (PI), area pulsed electron beams (PEE), raster scanned (RSEB) or multi - scanned electron beams (MSEB...where high quality or tailored profiles are required. Continuous wave lasers and multi -scanned or swept-line electron beams are the most likely candidates

On the use of SEM techniques to determine clockwise or counterclockwise P-T paths: insights from metapelites (Yunquera Unit, Betic Cordilleras)

NASA Astrophysics Data System (ADS)

Esteban, J. J.; Tubía, J. M.; Cuevas, J.; Gil Ibarguchi, J. I.

2012-04-01

Garnet porphyroblast textures and compositions, coupled to those of accompanying phases, are one of the most useful tools to determine the change of P-T conditions during metamorphism. This is currently done quantitatively through the use of conventional thermobarometry and pseudosection analysis, whose validity is conditioned by assumptions on the chemical mineral equilibrium (e.g. Spear, 1993). In the case of metapelites, the classic approach involves the use of core to rim compositions in zoned garnets and coexisting phases by electron microprobe analysis. Nonetheless, it is a high time consuming technique. As an alternative, we test the use of back-scattered electron (BSE) images and semi-quantitative energy-dispersive X-ray spectroscopy profiles obtained by scanning eletron microscope (SEM-EDX) to distinguish between clockwise and counterclockwise P-T paths. We applied these SEM techniques in samples of micaschist from the Yunquera Unit (Internal Zone, Betic Cordilleras, Spain) (Dürr, 1969). BSE images were obtained on selected areas covering the texturally and mineralogically most significant garnet-bearing portions, whereas semiquantitative profiles for Ca, Fe, Mg and Mn were obtained by means of EDX counting. Different types of chemical profiles were observed: (a) normal (growth) continuous zoning, (b) discontinuous, and (c) reverse continuous zoning. The patterns of chemical profiles are in agreement with changes in internal microstructures and density of inclusion. Two types of continuous growth zoning were identified in subspherical garnets bearing internal foliations. XMn and XFe ratios show the classical bell-shaped geometry while XCa increases in some cases and decreases in others towards rims. Discontinuous garnet profiles are typical of multistage garnet growth, which is outlined by the occurrence of alternating low- and high-inclusion density areas. Garnets with low-inclusion density cores show homogeneous core composition with an abrupt change towards the rims marked by a rapid increase in XCa and decrease in XFe and XMg ratios. Garnets with high-density inclusion cores depict XCa ratios at core similar to the previous ones and a sudden decrease towards the rims, whereas XFe and XMg continuously increase from core to rim. Reverse continuous profiles are typical of small idiomorphic garnets either enclosed or surrounding large muscovite porphyroblasts. These garnets show an increase in XMn and a decrease in XFe and XMg ratios from core to rim with minor variations in Ca. Taken as a whole, the chemical profiles reveal a generalized increase in Fe# [Fe/(Fe+Mg)] towards the rims that would attest to a temperature increase during the growth of the garnets. In addition, continuous and discontinuous variations in XCa ratios in large garnets suggest prograde garnet growth following a clockwise P-T path evolution, that is, a pressure increase followed by decrease under continuously increasing T conditions. As a conclusion, it is suggested that a method based mainly on the acquisition of BSE images and semiquantitative chemical profiles on selected minerals, and their interpretation using conventional thermo-barometric reasoning would be useful in the establishment of relative P-T paths that might help to save time and better identify the areas of interest for later detailed electron microprobe studies.

Scanning Transmission Electron Microscopy | Materials Science | NREL

Science.gov Websites

mode by collecting the EDS and EELS signals point-by-point as one scans the electron probe across the . Examples of Scanning Transmission Electron Microscopy Capabilities Z-contrast image microphoto taken by

Application of environmental scanning electron microscopy to determine biological surface structure.

PubMed

Kirk, S E; Skepper, J N; Donald, A M

2009-02-01

The use of environmental scanning electron microscopy in biology is growing as more becomes understood about the advantages and limitations of the technique. These are discussed and we include new evidence about the effect of environmental scanning electron microscopy imaging on the viability of mammalian cells. We show that although specimen preparation for high-vacuum scanning electron microscopy introduces some artefacts, there are also challenges in the use of environmental scanning electron microscopy, particularly at higher resolutions. This suggests the two technologies are best used in combination. We have used human monocyte-derived macrophages as a test sample, imaging their complicated and delicate membrane ruffles and protrusions. We have also explored the possibility of using environmental scanning electron microscopy for dynamic experiments, finding that mammalian cells cannot be imaged and kept alive in the environmental scanning electron microscopy. The dehydration step in which the cell surface is exposed causes irreversible damage, probably via loss of membrane integrity during liquid removal in the specimen chamber. Therefore, mammalian cells should be imaged after fixation where possible to protect against damage as a result of chamber conditions.

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.

The uniformity and imaging properties of some new ceramic scintillators

NASA Astrophysics Data System (ADS)

Chac, George T. L.; Miller, Brian W.; Shah, Kanai; Baldoni, Gary; Domanik, Kenneth J.; Bora, Vaibhav; Cherepy, Nerine J.; Seeley, Zachary; Barber, H. Bradford

2012-10-01

Results are presented of investigations into the composition, uniformity and gamma-ray imaging performance of new ceramic scintillators with synthetic garnet structure. The ceramic scintillators were produced by a process that uses flame pyrolysis to make nanoparticles which are sintered into a ceramic and then compacted by hot isostatic compression into a transparent material. There is concern that the resulting ceramic scintillator might not have the uniformity of composition necessary for use in gamma-ray spectroscopy and gamma-ray imaging. The compositional uniformity of four samples of three ceramic scintillator types (GYGAG:Ce, GLuGAG:Ce and LuAG:Pr) was tested using an electron microprobe. It was found that all samples were uniform in elemental composition to the limit of sensitivity of the microprobe (few tenths of a percent atomic) over distance scales from ~ 1 cm to ~ 1 um. The light yield and energy resolution of all ceramic scintillator samples were mapped with a highly collimated 57Co source (122 keV) and performance was uniform at mapping scale of 0.25 mm. Good imaging performance with single gamma-ray photon detection was demonstrated for all samples using a BazookaSPECT system, and the imaging spatial resolution, measured as the FWHM of a LSF was 150 um.

Jarosite in the Shergottite Que 94201

NASA Technical Reports Server (NTRS)

Ross, D. K.; Ito, M.; Rao, M. N.; Hervig, R.; Williams, L. B.; Nyquist, Laurence E.; Peslier, A.

2010-01-01

Veins of the hydroxylated, potassium ferric sulfate mineral jarosite - KFe3(SO4)2(OH)6 - have been identified in the martian meteorite Queen Alexandra Range (QUE) 94201. Iron potassium sulfate had been reported in QUE 94201 by Wentworth and Gooding. Jarosite has been reported in other Martian meteorites - Roberts Massif (RBT) 04262, Miller Range (MIL) 03346, and Yamato 000593 - and it has been identified on the Martian surface by Moessbauer spectroscopy. Given the presence of jarosite on Mars, and the burgeoning interest in water-rock interactions on Mars, the question arises whether jarosite in Martian meteorites is formed by aqueous alteration on Mars, or in Antarctica. Hydrogen isotopes are potentially sensitive indicators of the site of formation or last equilibration of hydrous alteration minerals, because of the large difference between D/H ratio of the Martian atmosphere (and also presumably the cryosphere) and terrestrial hydrogen. The Martian atmospheric delta D(sub SMOW) ratio is approximately +4200%o, igneous minerals with substantial hydrogen (phosphates) have high D, +2000%o to +4700%o versus terrestrial waters with approximately 480%o to +130%o. The crystal chemistry and structure of jarosite are reviewed in Papi ke et al. Here we report hydrogen isotopes measured in jarosite in QUE 94201 by ion microprobe, and also report on the major element composition of jarosite measured by electron microprobe.

Accurate Virus Quantitation Using a Scanning Transmission Electron Microscopy (STEM) Detector in a Scanning Electron Microscope

DTIC Science & Technology

2017-06-29

Accurate Virus Quantitation Using a Scanning Transmission Electron Microscopy (STEM) Detector in a Scanning Electron Microscope Candace D Blancett1...L Norris2, Cynthia A Rossi4 , Pamela J Glass3, Mei G Sun1,* 1 Pathology Division, United States Army Medical Research Institute of Infectious...Diseases (USAMRIID), 1425 Porter Street, Fort Detrick, Maryland, 21702 2Biostatistics Division, United States Army Medical Research Institute of

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

PubMed

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

2000-01-01

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

Microprobe investigation of brittle segregates in aluminum MIG and TIG welds

NASA Technical Reports Server (NTRS)

Larssen, P. A.; Miller, E. L.

1968-01-01

Quantitative microprobe analysis of segregated particles in aluminum MIG /Metal Inert Gas/ and TIG /Tungsten Inert Gas/ welds indicated that there were about ten different kinds of particles, corresponding to ten different intermetallic compounds. Differences between MIG and TIG welds related to the individual cooling rates of these welds.

U/Th dating by SHRIMP RG ion-microprobe mass spectrometry using single ion-exchange beads

NASA Astrophysics Data System (ADS)

Bischoff, James L.; Wooden, Joe; Murphy, Fred; Williams, Ross W.

2005-04-01

We present a new analytical method for U-series isotopes using the SHRIMP RG (Sensitive High mass Resolution Ion MicroProbe) mass spectrometer that utilizes the preconcentration of the U-series isotopes from a sample onto a single ion-exchange bead. Ion-microprobe mass spectrometry is capable of producing Th ionization efficiencies in excess of 2%. Analytical precision is typically better than alpha spectroscopy, but not as good as thermal ionization mass spectroscopy (TIMS) and inductively coupled plasma multicollector mass spectrometry (ICP-MS). Like TIMS and ICP-MS the method allows analysis of small samples sizes, but also adds the advantage of rapidity of analysis. A major advantage of ion-microprobe analysis is that U and Th isotopes are analyzed in the same bead, simplifying the process of chemical separation. Analytical time on the instrument is ˜60 min per sample, and a single instrument-loading can accommodate 15-20 samples to be analyzed in a 24-h day. An additional advantage is that the method allows multiple reanalyses of the same bead and that samples can be archived for reanalysis at a later time. Because the ion beam excavates a pit only a few μm deep, the mount can later be repolished and reanalyzed numerous times. The method described of preconcentrating a low concentration sample onto a small conductive substrate to allow ion-microprobe mass spectrometry is potentially applicable to many other systems.

U/Th dating by SHRIMP RG ion-microprobe mass spectrometry using single ion-exchange beads

USGS Publications Warehouse

Bischoff, J.L.; Wooden, J.; Murphy, F.; Williams, Ross W.

2005-01-01

We present a new analytical method for U-series isotopes using the SHRIMP RG (Sensitive High mass Resolution Ion MicroProbe) mass spectrometer that utilizes the preconcentration of the U-series isotopes from a sample onto a single ion-exchange bead. Ion-microprobe mass spectrometry is capable of producing Th ionization efficiencies in excess of 2%. Analytical precision is typically better than alpha spectroscopy, but not as good as thermal ionization mass spectroscopy (TIMS) and inductively coupled plasma multicollector mass spectrometry (ICP-MS). Like TIMS and ICP-MS the method allows analysis of small samples sizes, but also adds the advantage of rapidity of analysis. A major advantage of ion-microprobe analysis is that U and Th isotopes are analyzed in the same bead, simplifying the process of chemical separation. Analytical time on the instrument is ???60 min per sample, and a single instrument-loading can accommodate 15-20 samples to be analyzed in a 24-h day. An additional advantage is that the method allows multiple reanalyses of the same bead and that samples can be archived for reanalysis at a later time. Because the ion beam excavates a pit only a few ??m deep, the mount can later be repolished and reanalyzed numerous times. The method described of preconcentrating a low concentration sample onto a small conductive substrate to allow ion-microprobe mass spectrometry is potentially applicable to many other systems. Copyright ?? 2005 Elsevier Ltd.

A Seafloor Microbial Biome Hosted within Incipient Ferromanganese Crusts

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

Templeton, Alexis S.; Knowles, A. S.; Eldridge, D. L.

2009-11-15

Unsedimented volcanic rocks exposed on the seafloor at ridge systems and Seamounts host complex, abundant and diverse microbial communities that are relatively cosmopolitan in distribution (Lysnes, Thorseth et al. 2004; Mason, Stingl et al. 2007; Santelli, Orcutt et al. 2008). The most commonly held hypothesis is that the energy released by the hydration, dissolution and oxidative alteration of volcanic glasses in seawater drives the formation of an ocean crust biosphere (Thorseth, Furnes et al. 1992; Fisk, Giovannoni et al. 1998; Furnes and Staudigel 1999). The combined thermodynamically favorable weathering reactions could theoretically support anywhere from 105 to 109 cells/gram ofmore » rock depending upon the metabolisms utilized and cellular growth rates and turnover (Bach and Edwards 2003; Santelli, Orcutt et al. 2008). Yet microbially-mediated basalt alteration and energy conservation has not been directly demonstrated on the seafloor. By using synchrotron-based x-ray microprobe mapping, x-ray absorption spectroscopy and high-resolution scanning and transmission electron microscopy observations of young volcanic glasses recovered from the outer flanks of Loihi Seamount, we intended to identify the initial rates and mechanisms of microbial basalt colonization and bioalteration. Instead, here we show that microbial biofilms are intimately associated with ferromanganese crusts precipitating onto basalt surfaces from cold seawater. Thus we hypothesize that microbial communities colonizing seafloor rocks are established and sustained by external inputs of potential energy sources, such as dissolved and particulate Fe(II), Mn(II) and organic matter, rather than rock dissolution.« less

[In Situ Analysis of Element Geochemistry in Submarine Basalt in Hydrothermal Areas from Ultraslow Spreading Southwest Indian Ridge].

PubMed

Wang, Yan; Sun, Xiao-ming; Xu, Li; Liang, Ye-heng; Wu, Zhong-wei; Fu, Yu; Huang, Yi

2015-03-01

In this study, we analyze element geochemistry of submarine basalt in situ, which is sampled in hydrothermal areas from ultraslow spreading Southwest Indian Ridge, including the fresh basalt rocks (B19-9, B15-13) and altered basalt (B5-2). And we can confirm that altered mineral in B5-2 is celadonite by microscope and Raman Spectrum. Furthermore, amygdaloidal celadonites are analyzed by electron microprobe (EPMA) and EDS-line scanning. The results show that K-contents decrease and Na-contents increase from the core to the edge in these altered minerals, indicating the transition from celadonite to saponite. Celadonite is an altered minerals, forming in low temperature (< 50 degrees C) and oxidizing condition, while saponite form in low water/rock and more reducing condition. As a result, the transition from celadonite to saponite suggests environment change from oxidizing to reducing condition. Using the result of EPMA as internal standard, we can analyze rare earth elements (REE) in altered mineral in situ. Most of result show positive Eu anomaly (Δ(Eu)), indicating hydrothermal fluid transform from oxidizing to reducing, and reducing fluid rework on the early altered minerals. Comparison with REE in matrix feldspar both in altered and unaltered zoning, we find that reducing fluid can leach REE from the matrix feldspar, leading to lower total REE concentrations and positive Eu anomaly. So leaching process play an important role in hydrothermal system.

Mineralogical assemblages forming at hyperalkaline warm springs hosted on ultramafic rocks: A case study of Oman and Ligurian ophiolites

NASA Astrophysics Data System (ADS)

Chavagnac, Valérie; Ceuleneer, Georges; Monnin, Christophe; Lansac, Benjamin; Hoareau, Guilhem; Boulart, Cédric

2013-07-01

We report on the mineralogical assemblages found in the hyperalkaline springs hosted on Liguria and Oman ophiolites based on exhaustive X-ray diffraction and scanning electron microprobe analyses. In Liguria, hyperalkaline springs produce a thin brownish calcite precipitate that covers the bedrock due to the concomitant atmospheric CO2 uptake and neutralization of the hyperalkaline waters. No brucite and portlandite minerals are observed. The discharge of alkaline waters in Oman ophiolite forms white-orange precipitates. Calcium carbonate minerals (calcite and/or aragonite) are the most abundant and ubiquitous precipitates and are produced by the same mechanism as in Liguria. This process is observed as a thin surface crust made of rhombohedral calcite. Morphological features of aragonite vary from needle-, bouquet-, dumbbell-, spheroidal-like habitus according to the origin of carbon, temperature, and ionic composition of the hyperalkaline springs, and the biochemical and organic compounds. Brucite is observed both at hyperalkaline springs located at the thrust plane and at the paleo-Moho. The varying mixing proportions between the surface runoff waters and the hyperalkaline ones control brucite precipitation. The layered double hydroxide minerals occur solely in the vicinity of hyperalkaline springs emerging within the bedded gabbros. Finally, the dominant mineralogical associations we found in Oman (Ca-bearing carbonates and brucite) in a serpentinizing environment driven by the meteoric waters are surprisingly the same as those observed at the Lost City hydrothermal site in a totally marine environment.

On the distribution of uranium in hair: Non-destructive analysis using synchrotron radiation induced X-ray fluorescence microprobe techniques

NASA Astrophysics Data System (ADS)

Israelsson, A.; Eriksson, M.; Pettersson, H. B. L.

2015-06-01

In the present study the distribution of uranium in single human hair shafts has been evaluated using two synchrotron radiation (SR) based micro X-ray fluorescence techniques; SR μ-XRF and confocal SR μ-XRF. The hair shafts originated from persons that have been exposed to elevated uranium concentrations. Two different groups have been studied, i) workers at a nuclear fuel fabrication factory, exposed mainly by inhalation and ii) owners of drilled bedrock wells exposed by ingestion of water. The measurements were carried out on the FLUO beamline at the synchrotron radiation facility ANKA, Karlsruhe. The experiment was optimized to detect U with a beam size of 6.8 μm × 3 μm beam focus allowing detection down to ppb levels of U in 10 s (SR μ-XRF setup) and 70 s (SR confocal μ-XRF setup) measurements. It was found that the uranium was present in a 10-15 μm peripheral layer of the hair shafts for both groups studied. Furthermore, potential external hair contamination was studied by scanning of unwashed hair shafts from the workers. Sites of very high uranium signal were identified as particles containing uranium. Such particles, were also seen in complementary analyses using variable pressure electron microscope coupled with energy dispersive X-ray analyzer (ESEM-EDX). However, the particles were not visible in washed hair shafts. These findings can further increase the understanding of uranium excretion in hair and its potential use as a biomonitor.

Microscopic, chemical, and molecular-biological investigation of the decayed medieval stained window glasses of two Catalonian churches

PubMed Central

Piñar, Guadalupe; Garcia-Valles, Maite; Gimeno-Torrente, Domingo; Fernandez-Turiel, Jose Luis; Ettenauer, Jörg; Sterflinger, Katja

2013-01-01

We investigated the decayed historical church window glasses of two Catalonian churches, both under Mediterranean climate. Glass surfaces were studied by scanning electron microscopy (SEM), energy dispersive spectrometry (EDS), and X-ray diffraction (XRD). Their chemical composition was determined by wavelength-dispersive spectrometry (WDS) microprobe analysis. The biodiversity was investigated by molecular methods: DNA extraction from glass, amplification by PCR targeting the16S rRNA and ITS regions, and fingerprint analyses by denaturing gradient gel electrophoresis (DGGE). Clone libraries containing either PCR fragments of the bacterial 16S rDNA or the fungal ITS regions were screened by DGGE. Clone inserts were sequenced and compared with the EMBL database. Similarity values ranged from 89 to 100% to known bacteria and fungi. Biological activity in both sites was evidenced in the form of orange patinas, bio-pitting, and mineral precipitation. Analyses revealed complex bacterial communities consisting of members of the phyla Proteobacteria, Bacteroidetes, Firmicutes, and Actinobacteria. Fungi showed less diversity than bacteria, and species of the genera Cladosporium and Phoma were dominant. The detected Actinobacteria and fungi may be responsible for the observed bio-pitting phenomenon. Moreover, some of the detected bacteria are known for their mineral precipitation capabilities. Sequence results also showed similarities with bacteria commonly found on deteriorated stone monuments, supporting the idea that medieval stained glass biodeterioration in the Mediterranean area shows a pattern comparable to that on stone. PMID:24092957

Visualizing trace element distribution in quartz using cathodoluminescence, electron microprobe, and laser ablation-inductively coupled plasma-mass spectrometry

USGS Publications Warehouse

Rusk, Brian; Koenig, Alan; Lowers, Heather

2011-01-01

Cathodoluminescent (CL) textures in quartz reveal successive histories of the physical and chemical fluctuations that accompany crystal growth. Such CL textures reflect trace element concentration variations that can be mapped by electron microprobe or laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS). Trace element maps in hydrothermal quartz from four different ore deposit types (Carlin-type Au, epithermal Ag, porphyry-Cu, and MVT Pb-Zn) reveal correlations among trace elements and between trace element concentrations and CL textures. The distributions of trace elements reflect variations in the physical and chemical conditions of quartz precipitation. These maps show that Al is the most abundant trace element in hydrothermal quartz. In crystals grown at temperatures below 300 °C, Al concentrations may vary by up to two orders of magnitude between adjacent growth zones, with no evidence for diffusion. The monovalent cations Li, Na, and K, where detectable, always correlate with Al, with Li being the most abundant of the three. In most samples, Al is more abundant than the combined total of the monovalent cations; however, in the MVT sample, molar Al/Li ratios are ~0.8. Antimony is present in concentrations up to ~120 ppm in epithermal quartz (~200–300 °C), but is not detectable in MVT, Carlin, or porphyry-Cu quartz. Concentrations of Sb do not correlate consistently with those of other trace elements or with CL textures. Titanium is only abundant enough to be mapped in quartz from porphyry-type ore deposits that precipitate at temperatures above ~400 °C. In such quartz, Ti concentration correlates positively with CL intensity, suggesting a causative relationship. In contrast, in quartz from other deposit types, there is no consistent correlation between concentrations of any trace element and CL intensity fluctuations.

Sulfides from Martian and Lunar Basalts: Comparative Chemistry for Ni Co Cu and Se

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

J Papike; P Burger; C Shearer

2011-12-31

Here Mars and Moon are used as 'natural laboratories' with Moon displaying lower oxygen fugacities ({approx}IW-1) than Mars ({approx}IW to FMQ). Moon has lower concentrations of Ni and Co in basaltic melts than does Mars. The major sulfides are troilite (FeS) in lunar basalts and pyrrhotite (Fe{sub 1-x}S) in martian basalts. This study focuses on the concentrations of Ni, Co, Cu, and Se. We chose these elements because of their geochemical importance and the feasibility of analyzing them with a combination of synchrotron X-ray fluorescence (SXRF) and electron microprobe (EPMA) techniques. The selenium concentrations could only be analyzed, at highmore » precision, with SXRF techniques as they are <150 ppm, similar to concentrations seen in carbonaceous chondrites and interplanetary dust particles (IDPs). Nickel and Co are in higher concentrations in martian sulfides than lunar and are higher in martian olivine-bearing lithologies than olivine-free varieties. The sulfides in individual samples show very large ranges in concentration (e.g., Ni ranges from 50 000 ppm to <5 ppm). These large ranges are mainly due to compositional heterogeneities within individual grains due to diffusion and phase separation. Electron microprobe wavelength-dispersive (WDS) mapping of Ni, Co, and Cu show the diffusion trajectories. Nickel and Co have almost identical diffusion trajectories leading to the likely nucleation of pentlandite (Ni,Co,Fe){sub 9}S{sub 8}, and copper diffuses along separate pathways likely toward chalcopyrite nucleation sites (CuFeS{sub 2}). The systematics of Ni and Co in lunar and martian sulfides clearly distinguish the two parent bodies, with martian sulfides displaced to higher Ni and Co values.« less

Determination of the spinel group end-members based on electron microprobe analyses

NASA Astrophysics Data System (ADS)

Ferracutti, Gabriela R.; Gargiulo, M. Florencia; Ganuza, M. Luján; Bjerg, Ernesto A.; Castro, Silvia M.

2015-04-01

The spinel group minerals have been the focus of many studies, not only because of their economic interest, but also due to the fact that they are very useful as petrogenetic indicators. The application End-Members Generator (EMG) allows to establish, based on electron microprobe analyses (EMPA), the 19 end-members of the spinel group: MgAl2O4 (Spinel sensu stricto, s.s.), FeAl2O4 (Hercynite), MnAl2O4 (Galaxite), ZnAl2O4 (Gahnite), MgFe2O4 (Magnesioferrite), Fe3O4 (Magnetite), MnFe2O4 (Jacobsite), ZnFe2O4 (Franklinite), NiFe2O4 (Trevorite), MgCr2O4 (Magnesiochromite), FeCr2O4 (Chromite), MnCr2O4 (Manganochromite), ZnCr2O4 (Zincochromite), NiCr2O4 (Nichromite), MgV2O4 (Magnesiocoulsonite), FeV2O4 (Coulsonite), MnV2O4 (Vuorelainenite), Mg2TiO4 (Qandilite) and Fe2TiO4 (Ulvöspinel). EMG is an application that does not require an installation process and was created with the purpose of performing calculations to obtain: cation proportions (per formula unit, p.f.u.), end-members of the spinel group, redistribution proportions for the corresponding end-members in the Magnetite prism or Ulvöspinel prism and a data validation section to check the results. EMG accepts .csv data files and the results obtained can be used to represent a given dataset with the SpinelViz program or any other 2D and/or 3D graph plotting software.

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

Old friends in a new light: “SnSb” revisited

NASA Astrophysics Data System (ADS)

Norén, Lasse; Withers, Ray L.; Schmid, Siegbert; Brink, Frank J.; Ting, Valeska

2006-02-01

The binary pnictide 'SnSb' has been re-investigated using a combination of X-ray, synchrotron and electron diffraction as well as electron microprobe analysis. Its structure was found to be incommensurately modulated with an underlying rhombohedral parent structure of space group symmetry R3¯m (No. 166), unit cell parameters a=b=4.3251(4) Å, c=5.3376(6) Å in the hexagonal setting. The incommensurate primary modulation wave vector q=1.3109(9)ch* and the superspace group symmetry is R3¯m (0, 0, ˜1.311) (No. 166.1). The refinement of the incommensurate structure indicates that the satellite reflections arise from displacive shifts of presumably essentially pure Sn and Sb layers along the hexagonal c-axis, with increasing distance between the Sn-layers and decreasing distance between the Sb layers.

Matrix mineralogy of the Lance CO3 carbonaceous chondrite - A transmission electron microscope study

NASA Technical Reports Server (NTRS)

Keller, Lindsay P.; Buseck, Peter R.

1990-01-01

Results are presented on electron microprobe analyses of three CO chondrites, all of which are falls: Lance, Kainsaz, and Warrenton. The TEM mineralogy results of Lance chondrite show that Fe-rich matrix olivines have been altered to Fe-bearing serpentine and Fe(3+) oxide; matrix metal was also altered to produce Fe(3+) oxides, leaving the residual metal enriched in Ni. Olivine grains in Lance's matrix contain channels along their 100-line and 001-line directions; the formation and convergence of such channels resulted in a grain-size reduction of the olivine. A study of Kainsaz and Warrenton showed that these meteorites do not contain phyllosilicates in their matrices, although both contain Fe(3+) oxide between olivine grains. It is suggested that, prior to its alteration, Lance probably resembled Kainsaz, an unaltered CO3 chondrite.

Interfacial layers in high-temperature-oxidized NiCrAl

NASA Technical Reports Server (NTRS)

Larson, L. A.; Browning, R.; Poppa, H.; Smialek, J.

1983-01-01

The utility of Auger electron spectroscopy combined with ball cratering for depth analysis of oxide and diffusion layers produced in a Ni-14Cr-24Al alloy by oxidation in air at 1180 C for 25 hr is demonstrated. During postoxidation cooling, the oxide layers formed by this alloy spalled profusely. The remaining very thin oxide was primarily Cr2O3 with a trace of Ni. The underlying metal substrate exhibited gamma/gamma-prime and beta phases with a metallic interfacial layer which was similar to the bulk gamma/gamma-prime phase but slightly enriched in Cr and Al. These data are compared to electron microprobe results from a nominally identical alloy. The diffusion layer thickness is modelled with a simple mass balance equation and compared to recent results on the diffusion process in NiCrAl alloys.

The thermal and deformational history of apollo 15418, A partly shock-melted lunar breccia

USGS Publications Warehouse

Nord, G.L.; Christie, J.M.; Lally, J.S.; Heuer, A.H.

1977-01-01

A thermal and mechanical history of lunar gabbroic anorthosite 15418 (1140g) has been deduced from petrographic examination of both exterior and interior thin sections and electron microprobe analysis and transmission electron microscopy of interior thin sections. We suggest that the rock underwent two major shock events - an early brecciation and annealing that produced a recrystallized breccia, followed by a second shock event that melted the surface of the rock, vitrified the interior plagioclase and heavily deformed the mafic phases. This latter shock even was also followed by annealing which crystallized the shock-produced glass and promoted recovery and recrystallization of the deformed crystalline phases. The complex mechanical and thermal history of 15418 compared with other ANT suite rocks at Spur Crater suggests that it had a different provenance. ?? 1977 D. Reidel Publishing Company, Dordrecht-Holland.

An electron beam linear scanning mode for industrial limited-angle nano-computed tomography.

PubMed

Wang, Chengxiang; Zeng, Li; Yu, Wei; Zhang, Lingli; Guo, Yumeng; Gong, Changcheng

2018-01-01

Nano-computed tomography (nano-CT), which utilizes X-rays to research the inner structure of some small objects and has been widely utilized in biomedical research, electronic technology, geology, material sciences, etc., is a high spatial resolution and non-destructive research technique. A traditional nano-CT scanning model with a very high mechanical precision and stability of object manipulator, which is difficult to reach when the scanned object is continuously rotated, is required for high resolution imaging. To reduce the scanning time and attain a stable and high resolution imaging in industrial non-destructive testing, we study an electron beam linear scanning mode of nano-CT system that can avoid mechanical vibration and object movement caused by the continuously rotated object. Furthermore, to further save the scanning time and study how small the scanning range could be considered with acceptable spatial resolution, an alternating iterative algorithm based on ℓ 0 minimization is utilized to limited-angle nano-CT reconstruction problem with the electron beam linear scanning mode. The experimental results confirm the feasibility of the electron beam linear scanning mode of nano-CT system.

An electron beam linear scanning mode for industrial limited-angle nano-computed tomography

NASA Astrophysics Data System (ADS)

Wang, Chengxiang; Zeng, Li; Yu, Wei; Zhang, Lingli; Guo, Yumeng; Gong, Changcheng

2018-01-01

Nano-computed tomography (nano-CT), which utilizes X-rays to research the inner structure of some small objects and has been widely utilized in biomedical research, electronic technology, geology, material sciences, etc., is a high spatial resolution and non-destructive research technique. A traditional nano-CT scanning model with a very high mechanical precision and stability of object manipulator, which is difficult to reach when the scanned object is continuously rotated, is required for high resolution imaging. To reduce the scanning time and attain a stable and high resolution imaging in industrial non-destructive testing, we study an electron beam linear scanning mode of nano-CT system that can avoid mechanical vibration and object movement caused by the continuously rotated object. Furthermore, to further save the scanning time and study how small the scanning range could be considered with acceptable spatial resolution, an alternating iterative algorithm based on ℓ0 minimization is utilized to limited-angle nano-CT reconstruction problem with the electron beam linear scanning mode. The experimental results confirm the feasibility of the electron beam linear scanning mode of nano-CT system.

Imaging of endodontic biofilms by combined microscopy (FISH/cLSM - SEM).

PubMed

Schaudinn, C; Carr, G; Gorur, A; Jaramillo, D; Costerton, J W; Webster, P

2009-08-01

Scanning electron microscopy is a useful imaging approach for the visualization of bacterial biofilms in their natural environments including their medical and dental habitats, because it allows for the exploration of large surfaces with excellent resolution of topographic features. Most biofilms in nature, however, are embedded in a thick layer of extracellular matrix that prevents a clear identification of individual bacteria by scanning electron microscopy. The use of confocal laser scanning microscopy on the other hand in combination with fluorescence in situ hybridization enables the visualization of matrix embedded bacteria in multi-layered biofilms. In our study, fluorescence in situ hybridization/confocal laser scanning microscopy and scanning electron microscopy were applied to visualize bacterial biofilm in endodontic root canals. The resulting fluorescence in situ hybridization /confocal laser scanning microscopy and scanning electron microscopy and pictures were subsequently combined into one single image to provide high-resolution information on the location of hidden bacteria. The combined use of scanning electron microscopy and fluorescence in situ hybridization / confocal laser scanning microscopy has the potential to overcome the limits of each single technique.

Corrosion in Magnesium and a Magnesium Alloy

NASA Astrophysics Data System (ADS)

Akavipat, Sanay

Magnesium and a magnesium alloy (AZ91C) have been ion implanted over a range of ions energies (50 to 150 keV) and doses (1 x 10('16) to 2 x 10('17) ions/cm('2)) to modify the corrosion properties of the metals. The corrosion tests were done by anodic polarization in chloride -free and chloride-containing aqueous solutions of a borated -boric acid with a pH of 9.3. Anodic polarization measurements showed that some implantations could greatly reduce the corrosion current densities at all impressed voltages and also increased slightly the pitting potential, which indicated the onset of the chloride attack. These improvements in corrosion resistance were caused by boron implantations into both types of samples. However, iron implantations were found to improve only the magnesium alloy. To study the corrosion in more detail, Scanning Auger Microprobe Spectrometer (SAM), Scanning Electron Microscope (SEM) with an X-ray Energy Spectrometry (XES) attachment, and Transmission Electron Microscope (TEM) measurements were used to analyze samples before, after, and at various corrosion stages. In both the unimplanted pure magnesium and AZ91C samples, anodic polarization results revealed that there were three active corrosion stages (Stages A, C, and E) and two passivating stages (Stages B and D). Examination of Stages A and B in both types of samples showed that only a mild, generalized corrosion had occurred. In Stage C of the TD samples, a pitting breakdown in the initial oxide film was observed. In Stage C of the AZ91C samples, galvanic and intergranular attack around the Mg(,17)Al(,12) intermetallic islands and along the matrix grain boundaries was observed. Stage D of both samples showed the formation of a thick, passivating oxygen containing, probably Mg(OH)(,2) film. In Stage E, this film was broken down by pits, which formed due to the presence of the chloride ions in both types of samples. Stages A through D of the unimplanted samples were not seen in the boron or iron implanted samples. Instead one low current density passivating stage was formed, which was ultimately broken down by the chloride attack. It is believed that the implantation of boron modified the initial surface film to inhibit corrosion, whereas the iron implantation modified the intermetallic (Mg(,17)Al(,12)) islands to act as sacrificial anodes.

Sparse sampling and reconstruction for electron and scanning probe microscope imaging

DOEpatents

Anderson, Hyrum; Helms, Jovana; Wheeler, Jason W.; Larson, Kurt W.; Rohrer, Brandon R.

2015-07-28

Systems and methods for conducting electron or scanning probe microscopy are provided herein. In a general embodiment, the systems and methods for conducting electron or scanning probe microscopy with an undersampled data set include: driving an electron beam or probe to scan across a sample and visit a subset of pixel locations of the sample that are randomly or pseudo-randomly designated; determining actual pixel locations on the sample that are visited by the electron beam or probe; and processing data collected by detectors from the visits of the electron beam or probe at the actual pixel locations and recovering a reconstructed image of the sample.

Willy: A prize noble Ur-Fremdling - Its history and implications for the formation of Fremdlinge and CAI

NASA Technical Reports Server (NTRS)

Armstrong, J. T.; El Goresy, A.; Wasserburg, G. J.

1985-01-01

The structure and composition of Willy, a 150-micron-diameter Fremdling in CAI 5241 from the Allende meteorite, are investigated using optical, secondary-electron, and electron-backscatter microscopy and electron-microprobe analysis. The results are presented in diagrams, maps, tables, graphs, and micrographs and compared with those for other Allende Fremdlinge. Willy is found to have a concentric-zone structure comprising a complex porous core of magnetite, metal, sulfide, scheelite, and other minor phases; a compact magnetite-apatite mantle; a thin (20 microns or less) reaction-assemblage zone; and a dense outer rim of fassaite with minor spinel. A multistage formation sequence involving changes in T and fO2 and preceding the introduction of Willy into the CAI (which itself preceded CAI spinel and silicate formation) is postulated, and it is inferred from the apparent lack of post-capture recrystallization that Willy has not been subjected to temperatures in excess of 600 C and may represent the precursor material for many other Fremdlinge.

[Microanalytical identification of barium sulphate crystals in statoliths of Chara rhizoids (Ch. fragilis, desv.)].

PubMed

Schröter, K; Läuchli, A; Sievers, A

1975-01-01

In contrast to the statocytes of higher plants, in which amyloplasts function as statoliths, Chara-rhizoids contain statolith vacuoles filled with biocrystallites of BaSO4. This was revealed by qualitative and quantitative electron microprobe analysis, atomic absorption spectrophotometry and selected area electron diffraction. The barium sulphate crystallites are rods which are linearly composed of globular subunits approximately 7 nm in diameter.The electron optical evidence of the crystallites depends on the nature of the fixatives. Best structural preservation was observed after fixation in a buffered solution of glutaraldehyde plus acrolein without addition of heavy metals. OsO4 and particularly KMnO4 partially dissolve the biocrystallites as well as synthetic BaSO4. The crystal solubility must be taken into consideration when micrographs of such small crystallites are interpreted.The fact that BaSO4 is chemically very inert seems to exclude biochemical interactions of the statoliths with other cell components during graviperception. It favours the theory that only the mass of the statoliths is effective.

Scanning ultrafast electron microscopy.

PubMed

Yang, Ding-Shyue; Mohammed, Omar F; Zewail, Ahmed H

2010-08-24

Progress has been made in the development of four-dimensional ultrafast electron microscopy, which enables space-time imaging of structural dynamics in the condensed phase. In ultrafast electron microscopy, the electrons are accelerated, typically to 200 keV, and the microscope operates in the transmission mode. Here, we report the development of scanning ultrafast electron microscopy using a field-emission-source configuration. Scanning of pulses is made in the single-electron mode, for which the pulse contains at most one or a few electrons, thus achieving imaging without the space-charge effect between electrons, and still in ten(s) of seconds. For imaging, the secondary electrons from surface structures are detected, as demonstrated here for material surfaces and biological specimens. By recording backscattered electrons, diffraction patterns from single crystals were also obtained. Scanning pulsed-electron microscopy with the acquired spatiotemporal resolutions, and its efficient heat-dissipation feature, is now poised to provide in situ 4D imaging and with environmental capability.

Atom Optics for Bose-Einstein Condensates (BEC)

DTIC Science & Technology

2012-04-25

Electron Micrograph of the Top View of Test Chip A .......................................29 11. A Scanning Electron Micrograph of the Cross...Sectional View of Test Chip A .....................29 12. A Scanning Electron Micrograph of the Top View of Test Chip B...30 13. A Scanning Electron Micrograph of the Cross Sectional View of Test Chip B .....................30 14. Toner Masks for Etching

Speciation of PM10 sources of airborne nonferrous metals within the 3-km zone of lead/zinc smelters.

PubMed

Batonneau, Yann; Bremard, Claude; Gengembre, Leon; Laureyns, Jacky; Le Maguer, Agnes; Le Maguer, Didier; Perdrix, Esperanza; Sobanska, Sophie

2004-10-15

The purpose of this study was to estimate the speciation of PM10 sources of airborne Pb, Zn, and Cd metals (PM10 is an aerosol standard of aerodynamic diameter less than 10 microm.) in the atmosphere of a 3 km zone surrounding lead/zinc facilities in operation for a century. Many powdered samples were collected in stacks of working units (grilling, furnace, and refinery), outdoor storages (ores, recycled materials), surrounding waste slag (4 Mt), and polluted topsoils (3 km). PM10 samples were generated from the raw powders by using artificial resuspension and collection devices. The bulk PM10 multielemental analyses were determined by inductively coupled plasma-atomic emission spectrometry (ICP-AES). The proportions in mass of Pb (50%), Zn (40%), and Cd (1%) contents and associated metals (traces) reach the proportions of corresponding raw powdered samples of ores, recycled materials, and fumesize emissions of plants without specific enrichment. In contrast, Pb (8%) and Zn (15%) contents of PM10 of slag deposit were found to be markedly higher than those of raw dust, Pb (4%), and Zn (9%), respectively. In the same way, Pb (0.18%), Zn (0.20%), and Cd (0.004%) were enriched by 1.7, 2.1, and 2.3 times, respectively, in PM10 as compared with raw top-soil corresponding values. X-ray wavelength dispersive electron-microprobe (EM-WDS) microanalysis did not indicate well-defined phases or simple stoichiometries of all the PM10 samples atthe level of the spatial resolution (1 microm3). X-ray photoelectron spectroscopy (XPS) indicated that minor elements such as Cd, Hg, and C are more concentrated on the particle surface than in the bulk of PM10 generated by the smelting processes. (XPS) provided also the average speciation of the surface of PM10; Pb is mainly represented as PbSO4, Zn as ZnS, and Cd as CdS or CdSO4, and small amounts of coke were also detected. The speciation of bulk PM10 crystallized compounds was deduced from XRD diffractograms with a raw estimation of the relative quantities. PbS and ZnS were found to be the major phases in PM10 generated by the smelting facilities with PbSO4, PbSO4 x PbO, PbSO4 x 4PbO, Pb metal, and ZnO as minor phases. The slag waste PM10 was found to contain some amounts of PbCO3, PbSO4 x PbO, and ZnFe2O4 phases. The large heterogeneity at the level of the individual particle generates severe overlap of chemical information even at the microm scale using electron microprobe (WDS) and Raman microprobe techniques. Fortunately, scanning Raman microspectrometry combined with SIMPle-to-use Interactive Self-modeling Mixture Analysis (SIMPLISMA) performed the PM10 speciation at the level of individual particles. The speciation of major Pb, Zn, and Cd compounds of PM10 stack emissions and wind blown dust of ores and recycled materials were found to be PbSO4, PbSO4 x PbO, PbSO4 x 4PbO, PbO, metallic Pb, ZnS, ZnO, and CdS. The PM10 dust of slag waste was found to contain PbCO3, Pb(OH)2 x 2PbCO3, PbSO4 x PbO, and ZnS, while PM10-bound Pb, Zn of the top-soils contain Pb5(PO4)3Cl, ZnFe2O4 as well as Pb(II) and Zn(II) compounds adsorbed on Fe(III) oxides and in association with clays.

Method and apparatus for a high-resolution three dimensional confocal scanning transmission electron microscope

DOEpatents

de Jonge, Niels [Oak Ridge, TN

2010-08-17

A confocal scanning transmission electron microscope which includes an electron illumination device providing an incident electron beam propagating in a direction defining a propagation axis, and a precision specimen scanning stage positioned along the propagation axis and movable in at least one direction transverse to the propagation axis. The precision specimen scanning stage is configured for positioning a specimen relative to the incident electron beam. A projector lens receives a transmitted electron beam transmitted through at least part of the specimen and focuses this transmitted beam onto an image plane, where the transmitted beam results from the specimen being illuminated by the incident electron beam. A detection system is placed approximately in the image plane.

Mach 1 oxidation of thoriated nickel chromium at 1204 C (2200 F)

NASA Technical Reports Server (NTRS)

Lowell, C. E.; Sanders, W. A.

1971-01-01

TD NiCr was exposed to a Mach 1, 1-atmosphere gas stream at 1204 C for times up to 50 hours. Weight change, metal thickness loss, X-ray diffraction, metallographic, and electron microprobe analyses were made. Neither surface preparation nor thermal cycling had an appreciable effect on the results. Initially, Cr2O3 formed and volatilized, allowing a rapid metal loss rate of 40 microns per hour. After about 1 hour the Cr2O3 broke down, resulting in an NiO overgrowth. The metal loss rate then slowed to 2.5 microns per hour and remained constant to 50 hours.

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.

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.

The effect of microstructure on the fracture toughness of titanium alloys

NASA Technical Reports Server (NTRS)

Vanstone, R. H.; Low, J. R., Jr.; Shannon, J. L., Jr.

1974-01-01

The microstructure of the alpha titanium alloy Ti-5Al-2.5Sn and the metastable beta titanium alloy Beta 3 was examined. The material was from normal and extra low interstitial grade plates which were either air-cooled or furnace-cooled from an annealing treatment. Beta 3 was studied in alpha-aged and omega-aged plates which were heat treated to similar strength levels. Tensile and plane strain fracture toughness tests were conducted at room temperature on the alpha-aged material. The microstructure and fracture mechanisms of alloys were studied using optical metallography, electron microscopy, microprobe analyses, and texture pole figures. Future experiments are described.

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.)

Some aspects of the thermal history of lunar glass.

NASA Technical Reports Server (NTRS)

Cooper, A. R.; Varshneya, A. K.; Sarkar, S. K.; Swift, J.; Klein, L.; Yen, F.

1972-01-01

Electron microprobe examination revealed that glassy lunar fragments had inclusions as well as boundaries between mineral glasses of different compositions. Glassy lunar spherules showed detectable heterogeneity less marked than that of the fragments. The room-temperature refractive indices and densities of the spherules are changed by heat-treating them at 500 to 700 C. The large increases (as much as 2% in density and 0.7% in index of refraction) are difficult to explain on the basis of classical glass-transition phenomena alone unless extremely rapid cooling rates are assumed. Further, the spherules darkened significantly when they were heated in air or a medium vacuum above 625 C.

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.

SPE-LEEM Studies on the Surface and Electronic Structure of 2-D Transition Metal Dichalcogenides (Part II)

NASA Astrophysics Data System (ADS)

Jin, Wencan; Yeh, Po-Chun; Zaki, Nader; Zhang, Datong; Sadowski, Jerzy; Al-Mahboob, Abdullah; van de Zande, Arend; Chenet, Daniel; Dadap, Jerry; Herman, Irving; Sutter, Peter; Hone, James; Osgood, Richard

2014-03-01

In this work, we studied the surface and electronic structure of monolayer and few-layer exfoliated MoS2 and WSe2, as well as chemical-vapor-deposition (CVD) grown MoS2, using Spectroscopic Photoemission and Low Energy Electron Microscope (SPE-LEEM). LEEM measurements reveal that, unlike exfoliated MoS2, CVD-grown MoS2 exhibits grain-boundary alterations due to surface strain. However, LEEM and micro-probe low energy electron diffraction show that the quality of CVD-grown MoS2 is comparable to that of exfoliated MoS2. Micrometer-scale angle-resolved photoemission spectroscopy (ARPES) measurement on exfoliated MoS2 and WSe2 single-crystals provides direct evidence for the shifting of the valence band maximum from Γ to K, when the layer number is thinned down to one, as predicted by density functional theory. Our measurements of the k-space resolved electronic structure allow for further comparison with other theoretical predictions and with transport measurements. This work is supported by DOE grant DE-FG 02-04-ER-46157, research carried out in part at the CFN and NSLS, Brookhaven National Laboratory.

Atmospheric scanning electron microscope observes cells and tissues in open medium through silicon nitride film.

PubMed

Nishiyama, Hidetoshi; Suga, Mitsuo; Ogura, Toshihiko; Maruyama, Yuusuke; Koizumi, Mitsuru; Mio, Kazuhiro; Kitamura, Shinichi; Sato, Chikara

2010-03-01

Direct observation of subcellular structures and their characterization is essential for understanding their physiological functions. To observe them in open environment, we have developed an inverted scanning electron microscope with a detachable, open-culture dish, capable of 8 nm resolution, and combined with a fluorescence microscope quasi-simultaneously observing the same area from the top. For scanning electron microscopy from the bottom, a silicon nitride film window in the base of the dish maintains a vacuum between electron gun and open sample dish while allowing electrons to pass through. Electrons are backscattered from the sample and captured by a detector under the dish. Cells cultured on the open dish can be externally manipulated under optical microscopy, fixed, and observed using scanning electron microscopy. Once fine structures have been revealed by scanning electron microscopy, their component proteins may be identified by comparison with separately prepared fluorescence-labeled optical microscopic images of the candidate proteins, with their heavy-metal-labeled or stained ASEM images. Furthermore, cell nuclei in a tissue block stained with platinum-blue were successfully observed without thin-sectioning, which suggests the applicability of this inverted scanning electron microscope to cancer diagnosis. This microscope visualizes mesoscopic-scale structures, and is also applicable to non-bioscience fields including polymer chemistry. (c) 2010 Elsevier Inc. 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.

Bioaccumulation of chromium in aquatic macrophyte Borreria scabiosoides Cham. & Schltdl.

NASA Astrophysics Data System (ADS)

Mangabeira, P. A.; Mielke, M. S.; Arantes, I.; Dutruch, L.; Silva, D. da. C.; Barbier, F.; de Almeida, A.-A. F.; Oliveira, A. H.; Severo, M. I. G.; Labejof, L.; Rocha, D. C.; Rosa, T. S.; Santana, K. B.; Gavrilov, K. L.; Galle, P.; Levi-Setti, R.; Grenier-Loustalot, M. F.

2006-07-01

The capacity of Borreria scabiosoides Cham. & Schltdl. growing in hydroponics solutions to remove Cr (III) from water was evaluated. This macrophytes efficiently removed Cr from water at concentrations of 25 and 50 mg/l Cr -1. High resolution imaging secondary ion mass-spectrometry (HRI-SIMS) measurements were performed using scanning ion microprobe at the University of Chicago (UC-SIM). The inductively coupled plasma sector type mass spectrometer (HR-ICP-MS) was used to analyse all samples. In general, plant roots exhibited higher metal concentrations than the aerial plants parts. Borreria shows promise for the removal and store Cr from contaminated wastewater. The ion images demonstrated that Cr is preferentially accumulated in cell walls and in some vacuoles of cortical roots cells. The number of Cr deposits are higher in cortical parenchyma, particularly in vacuoles and cell walls, compared to stellar tissue.

Carbon-11 labelling of 8[[3-[4-(2-[(11)C]methoxyphenyl)piperazin-1-yl]-2-hydroxypropyl]oxy]thiochroman, a presynaptic 5-HT(1A) receptor agonist, and its in vivo evaluation in anaesthetised rat and in awake cat.

PubMed

Zimmer, Luc; Fournet, Guy; Benoît, Joseph; Guillaumet, Gérald; Le Bars, Didier

2003-07-01

A new compound, 8[[3-[4-(2-[(11)C]methoxyphenyl)piperazin-1-yl]-2-hydroxypropyl]oxy]thiochroman was labeled via O-methylation with [(11)C]methyl iodide in good yield and specific activity. Original biological evaluations included (i) the study in anesthetized rat with a beta-sensitive intracerebral probe (beta-Microprobe), allowing to measure locally the kinetic of the new PET ligand, and (ii) a PET-scan on a conditioned cat maintained awake during the acquisition. In both in vivo techniques, the new ligand did not reveal any specific binding in hippocampus indicating that this radiotracer is not suitable for mapping 5HT(1A) receptors using positron emission tomography.

Electronic noise in CT detectors: Impact on image noise and artifacts.

PubMed

Duan, Xinhui; Wang, Jia; Leng, Shuai; Schmidt, Bernhard; Allmendinger, Thomas; Grant, Katharine; Flohr, Thomas; McCollough, Cynthia H

2013-10-01

The objective of our study was to evaluate in phantoms the differences in CT image noise and artifact level between two types of commercial CT detectors: one with distributed electronics (conventional) and one with integrated electronics intended to decrease system electronic noise. Cylindric water phantoms of 20, 30, and 40 cm in diameter were scanned using two CT scanners, one equipped with integrated detector electronics and one with distributed detector electronics. All other scanning parameters were identical. Scans were acquired at four tube potentials and 10 tube currents. Semianthropomorphic phantoms were scanned to mimic the shoulder and abdominal regions. Images of two patients were also selected to show the clinical values of the integrated detector. Reduction of image noise with the integrated detector depended on phantom size, tube potential, and tube current. Scans that had low detected signal had the greatest reductions in noise, up to 40% for a 30-cm phantom scanned using 80 kV. This noise reduction translated into up to 50% in dose reduction to achieve equivalent image noise. Streak artifacts through regions of high attenuation were reduced by up to 45% on scans obtained using the integrated detector. Patient images also showed superior image quality for the integrated detector. For the same applied radiation level, the use of integrated electronics in a CT detector showed a substantially reduced level of electronic noise, resulting in reductions in image noise and artifacts, compared with detectors having distributed electronics.

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.

Quantitative analysis of domain texture in polycrystalline barium titanate by polarized Raman microprobe spectroscopy

NASA Astrophysics Data System (ADS)

Sakashita, Tatsuo; Chazono, Hirokazu; Pezzotti, Giuseppe

2007-12-01

A quantitative determination of domain distribution in polycrystalline barium titanate (BaTiO3, henceforth BT) ceramics has been pursued with the aid of a microprobe polarized Raman spectrometer. The crystallographic texture and domain orientation distribution of BT ceramics, which switched upon applying stress according to ferroelasticity principles, were determined from the relative intensity of selected phonon modes, taking into consideration a theoretical analysis of the angular dependence of phonon mode intensity for the tetragonal BT phase. Furthermore, the angular dependence of Raman intensity measured in polycrystalline BT depended on the statistical distribution of domain angles in the laser microprobe, which was explicitly taken into account in this work for obtaining a quantitative analysis of domain orientation for in-plane textured BT polycrystalline materials.

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.

Scanning ultrafast electron microscopy

PubMed Central

Yang, Ding-Shyue; Mohammed, Omar F.; Zewail, Ahmed H.

2010-01-01

Progress has been made in the development of four-dimensional ultrafast electron microscopy, which enables space-time imaging of structural dynamics in the condensed phase. In ultrafast electron microscopy, the electrons are accelerated, typically to 200 keV, and the microscope operates in the transmission mode. Here, we report the development of scanning ultrafast electron microscopy using a field-emission-source configuration. Scanning of pulses is made in the single-electron mode, for which the pulse contains at most one or a few electrons, thus achieving imaging without the space-charge effect between electrons, and still in ten(s) of seconds. For imaging, the secondary electrons from surface structures are detected, as demonstrated here for material surfaces and biological specimens. By recording backscattered electrons, diffraction patterns from single crystals were also obtained. Scanning pulsed-electron microscopy with the acquired spatiotemporal resolutions, and its efficient heat-dissipation feature, is now poised to provide in situ 4D imaging and with environmental capability. PMID:20696933

Elemental micro-PIXE mapping of hypersensitive lesions in Lagenaria sphaerica (Cucurbitaceae) resistant to Sphaerotheca fuliginea (powdery mildew)

NASA Astrophysics Data System (ADS)

Weiersbye-Witkowski, I. M.; Przybylowicz, W. J.; Straker, C. J.; Mesjasz-Przybylowicz, J.

1997-07-01

Genotypes of the Southern African cucurbit, Lagenaria sphaerica, that are resistant to powdery-mildew ( Sphaerotheca fuliginea) exhibit foliar hypersensitive (HS) lesions on inoculation with this fungal pathogen. Elemental distributions across radially symmetrical HS lesions, surrounding unlesioned leaf tissue and uninoculated leaf tissue, were obtained using the true elemental imaging system (Dynamic Analysis) of the NAC Van de Graaff nuclear microprobe. Raster scans of 3 MeV protons were complemented by simultaneous PIXE and BS point analyses. The composition of cellulose (C 6H 10O 5) was used as constant matrix composition for scans, and the sample thickness was found from BS spectra. Si and elements heavier than Ca contributed to matrix composition within HS lesions and the locally elevated Ca raised the limits of detection for some trace metals of interest. In comparison to uninoculated tissue, inoculated tissue was characterised by higher overall concentrations of all measured elements except Cu. Fully developed, 6 day-old HS lesions and the surrounding tissue could be divided into five zones, centred on the fungal infection site. Each zone was characterized by distinct local elemental distributions (either depletion, or accumulation to potentially phytotoxic levels).

Scanning transmission ion microscopy mass measurements for quantitative trace element analysis within biological samples and validation using atomic force microscopy thickness measurements

NASA Astrophysics Data System (ADS)

Devès, Guillaume; Cohen-Bouhacina, Touria; Ortega, Richard

2004-10-01

We used the nuclear microprobe techniques, micro-PIXE (particle-induced X-ray emission), micro-RBS (Rutherford backscattering spectrometry) and scanning transmission ion microscopy (STIM) in order to perform the characterization of trace element content and spatial distribution within biological samples (dehydrated cultured cells, tissues). The normalization of PIXE results was usually expressed in terms of sample dry mass as determined by micro-RBS recorded simultaneously to micro-PIXE. However, the main limit of RBS mass measurement is the sample mass loss occurring during irradiation and which could be up to 30% of the initial sample mass. We present here a new methodology for PIXE normalization and quantitative analysis of trace element within biological samples based on dry mass measurement performed by mean of STIM. The validation of STIM cell mass measurements was obtained in comparison with AFM sample thickness measurements. Results indicated the reliability of STIM mass measurement performed on biological samples and suggested that STIM should be performed for PIXE normalization. Further information deriving from direct confrontation of AFM and STIM analysis could as well be obtained, like in situ measurements of cell specific gravity within cells compartment (nucleolus and cytoplasm).

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.

A multi-component evaporation model for beam melting processes

NASA Astrophysics Data System (ADS)

Klassen, Alexander; Forster, Vera E.; Körner, Carolin

2017-02-01

In additive manufacturing using laser or electron beam melting technologies, evaporation losses and changes in chemical composition are known issues when processing alloys with volatile elements. In this paper, a recently described numerical model based on a two-dimensional free surface lattice Boltzmann method is further developed to incorporate the effects of multi-component evaporation. The model takes into account the local melt pool composition during heating and fusion of metal powder. For validation, the titanium alloy Ti-6Al-4V is melted by selective electron beam melting and analysed using mass loss measurements and high-resolution microprobe imaging. Numerically determined evaporation losses and spatial distributions of aluminium compare well with experimental data. Predictions of the melt pool formation in bulk samples provide insight into the competition between the loss of volatile alloying elements from the irradiated surface and their advective redistribution within the molten region.

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.

Microbial pathways and palaeoenvironmental conditions involved in the formation of phosphorite grains, Safaga District, Egypt

NASA Astrophysics Data System (ADS)

Salama, Walid; El-Kammar, Ahmed; Saunders, Martin; Morsy, Rania; Kong, Charlie

2015-07-01

Phosphatic grains of the shallow marine phosphorite deposits of Egypt are classified as either phosphatic bioclasts preserving biological structure (e.g. skeletal fragments such as fish bones and teeth) or phosphatic peloids and intraclasts. This study describes the destructive and constructive microbial pathways represented by bioerosion of bones by endolithic cyanobacteria and accretion of phosphatic peloids by bacteria. The palaeoenvironmental conditions and post-depositional/diagenetic history of these grains have also been considered. Scanning and transmission electron microscopy showed that the phosphatic peloids under transmitted light microscopy are composed mainly of microspheres (0.5 to 2.5 μm) similar in shape and size to coccoid-like bacteria. Chemical mapping showed that these microspheres are composed of carbonate-fluorapatite (CFA) and surrounded by degraded carbonaceous matrix. These grains are suggested to be reworked from pre-existing microbial mats during transgressive-regressive cycles affecting the southern Tethyan Campanian-Maastrichtian shallow continental shelf. The bioerosion of phosphatic bones is characterized by a network of meandering microborings that penetrated inward from the bone surface by endolithic cyanobacteria. The bioerosion of bones resulted in a gradual centripetal digestion and conversion of bones into micritic phosphate peloids. The bioerosion mechanism is probably started in the acidic sheath surrounding cyanobacteria followed by supersaturation of PO4 and reprecipitation of crystalline CFA as electron dense remineralized rims. Electron microprobe microanalyses showed that the remineralized microbored areas are higher in CaO, P2O5, and F and depleted in Cl, relative to unaltered bones. A gradual demineralization of remineralized rims followed by dissolution of cyanobacterial cells is probably occurred during diagenesis and meteoric water alteration leaving behind empty microborings. Bone exposed to meteoric water alteration is lower in CaO and P2O5 and higher in F and Cl than the unaltered bones. Understanding bone bioerosion has significant implications for palaeoenvironmental and taphonomic reconstruction, archaeological applications and a regional correlation of the late Cretaceous to Palaeogene phosphogenic province extending from Middle East to North Africa.

Fragmentation and growth processes in ultramafic pseudotachylites and associated wall rocks from Alpine Corsica

NASA Astrophysics Data System (ADS)

Dunkel, K.; Austrheim, H.; Plümper, O.; Ildefonse, B.; Ohl, M.; Jamtveit, B.

2017-12-01

Pseudotachylites, often taken as indicators of seismic slip, can form by comminution and/or melting. How the seismic energy released during a pseudotachylite-generating earthquake affects the wall rock surrounding the fault plane is not well known, although damage of the wall rock can have a substantial influence on the rheological properties of the rock and therefore on its further deformation and metamorphism. Micro- and nanostructures of pseudotachylites and their wall rocks in peridotites from Alpine Corsica have been characterized using optical, scanning and transmission electron microscopy, electron backscatter diffraction, and electron microprobe analysis. Pseudotachylites in dunites from the Cima di Gratera area in Cape Corse show a combination of comminution and melting. Olivine in the pseudotachylites is dislocation-rich whereas pyroxene is almost free of dislocations, indicating a fragmentation of the olivine during seismic slip and incomplete melting. The temperature pulse that induced melting was likely short-lived, since evidence for recovery in olivine is limited. Olivines in the wall rocks show a similarly high dislocation density and are strongly fragmented without being sheared. A fragmentation without shear strain, comparable to the "pulverization" described from shallower earthquakes, can probably only be explained by a high stress pulse released during a seismic event. Previous observations from the same area describe a transition from cataclastic wall rocks over mylonites and ultramylonites to pseudotachylite. This was taken as an indication that cataclasis weakened the rock and finally, in connection with thermal runaway, allowed for seismic slip. This difference between previous observations and those described here may be explained by a spatial heterogeneity in the deformation conditions. While earthquakes may have nucleated by self-localizing thermal runaway in cataclastic zones, they propagated also through previously undeformed rocks, causing fragmentation and partial melting at high stress. The fragmentation of the wall rock, whether it occurred by brittle or crystal-plastic mechanisms, allowed for the infiltration of fluids. Thus, earthquakes cause not only a physical, but also a chemical alteration of the wall rocks surrounding the fault plane

Scanning electron microscopy of hepatic ultrastructure: secondary, backscattered, and transmitted electron imaging.

PubMed

Miyai, K; Abraham, J L; Linthicum, D S; Wagner, R M

1976-10-01

Several methods of tissue preparation and different modes of operation of the scanning electron microscope were used to study the ultrastructure of rat liver. Rat livers were perfusion fixed with buffered 2 per cent paraformaldehyde or a mixture of 1.5 per cent paraformaldehyde and 1 per cent glutaraldehyde and processed as follows. Tissue blocks were postfixed in buffered 2 per cent osmium tetroxide followed sequentially by the ligand-mediated osmium binding technique, dehydration and cryofracture in ethanol, and critical point drying. They were then examined without metal coating in the scanning electron microscope operating in the secondary electron and backscattered electron modes. Fifty-micrometer sections were cut with a tissue sectioner, stained with lead citrate, postfixed with osmium, dehydrated, critical point dried, and examined in the secondary electron and back-scattered electron modes. Frozen sections (0.25 to 0.75 mum. thick) were cut by the method of Tokuyasu (Toluyasu KT: J Cell Biol 57:551, 1973) and their scanning transmission electron microscope images were examined either with a scanning transmission electron microscope detector or with a conversion stub using the secondary electron detector. Secondary electron images of the liver prepared by ligand-mediated osmium binding and subsequent cryofracture revealed such intracellular structures as cisternae of the endoplasmic reticulum, lysosomes, mitochondria, lipid droplets, nucleolus and nuclear chromatin, as well as the usual surface morphology, Lipocytes in the perisinusoidal space were readily identified. Backscattered electron images. Unembedded frozen sections had little drying artifact and were virtually free of freezing damage. The scanning transmission electron microscope image revealed those organelles visualized by the secondary electron mode in the ligand-mediated osmium binding-treated tissue.

Characterization of two-dimensional hexagonal boron nitride using scanning electron and scanning helium ion microscopy

NASA Astrophysics Data System (ADS)

Guo, Hongxuan; Gao, Jianhua; Ishida, Nobuyuki; Xu, Mingsheng; Fujita, Daisuke

2014-01-01

Characterization of the structural and physical properties of two-dimensional (2D) materials, such as layer number and inelastic mean free path measurements, is very important to optimize their synthesis and application. In this study, we characterize the layer number and morphology of hexagonal boron nitride (h-BN) nanosheets on a metallic substrate using field emission scanning electron microscopy (FE-SEM) and scanning helium ion microscopy (HIM). Using scanning beams of various energies, we could analyze the dependence of the intensities of secondary electrons on the thickness of the h-BN nanosheets. Based on the interaction between the scanning particles (electrons and helium ions) and h-BN nanosheets, we deduced an exponential relationship between the intensities of secondary electrons and number of layers of h-BN. With the attenuation factor of the exponential formula, we calculate the inelastic mean free path of electrons and helium ions in the h-BN nanosheets. Our results show that HIM is more sensitive and consistent than FE-SEM for characterizing the number of layers and morphology of 2D materials.

Electron beams scanning: A novel method

NASA Astrophysics Data System (ADS)

Askarbioki, M.; Zarandi, M. B.; Khakshournia, S.; Shirmardi, S. P.; Sharifian, M.

2018-06-01

In this research, a spatial electron beam scanning is reported. There are various methods for ion and electron beam scanning. The best known of these methods is the wire scanning wherein the parameters of beam are measured by one or more conductive wires. This article suggests a novel method for e-beam scanning without the previous errors of old wire scanning. In this method, the techniques of atomic physics are applied so that a knife edge has a scanner role and the wires have detector roles. It will determine the 2D e-beam profile readily when the positions of the scanner and detectors are specified.

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)

Reprint of: Atmospheric scanning electron microscope observes cells and tissues in open medium through silicon nitride film.

PubMed

Nishiyama, Hidetoshi; Suga, Mitsuo; Ogura, Toshihiko; Maruyama, Yuusuke; Koizumi, Mitsuru; Mio, Kazuhiro; Kitamura, Shinichi; Sato, Chikara

2010-11-01

Direct observation of subcellular structures and their characterization is essential for understanding their physiological functions. To observe them in open environment, we have developed an inverted scanning electron microscope with a detachable, open-culture dish, capable of 8 nm resolution, and combined with a fluorescence microscope quasi-simultaneously observing the same area from the top. For scanning electron microscopy from the bottom, a silicon nitride film window in the base of the dish maintains a vacuum between electron gun and open sample dish while allowing electrons to pass through. Electrons are backscattered from the sample and captured by a detector under the dish. Cells cultured on the open dish can be externally manipulated under optical microscopy, fixed, and observed using scanning electron microscopy. Once fine structures have been revealed by scanning electron microscopy, their component proteins may be identified by comparison with separately prepared fluorescence-labeled optical microscopic images of the candidate proteins, with their heavy-metal-labeled or stained ASEM images. Furthermore, cell nuclei in a tissue block stained with platinum-blue were successfully observed without thin-sectioning, which suggests the applicability of this inverted scanning electron microscope to cancer diagnosis. This microscope visualizes mesoscopic-scale structures, and is also applicable to non-bioscience fields including polymer chemistry. Copyright © 2010 Elsevier Inc. All rights reserved.

Petrography and microanalysis of Pennsylvanian coal-ball concretions (Herrin Coal, Illinois Basin, USA): Bearing on fossil plant preservation and coal-ball origins

NASA Astrophysics Data System (ADS)

Siewers, Fredrick D.; Phillips, Tom L.

2015-11-01

Petrographic analyses of 25 coal balls from well-studied paleobotanical profiles in the Middle Pennsylvanian Herrin Coal (Westphalian D, Illinois Basin) and five select coal balls from university collections, indicate that Herrin Coal-ball peats were permineralized by fibrous and non-fibrous carbonates. Fibrous carbonates occur in fan-like to spherulitic arrays in many intracellular (within tissue) pores, and are best developed in relatively open extracellular (between plant) pore spaces. Acid etched fibrous carbonates appear white under reflected light and possess a microcrystalline texture attributable to abundant microdolomite. Scanning electron microscopy, X-ray diffraction, and electron microprobe analysis demonstrate that individual fibers have a distinct trigonal prism morphology and are notable for their magnesium content (≈ 9-15 mol% MgCO3). Non-fibrous carbonates fill intercrystalline spaces among fibers and pores within the peat as primary precipitates and neomorphic replacements. In the immediate vicinity of plant cell walls, non-fibrous carbonates cut across fibrous carbonates as a secondary, neomorphic phase attributed to coalification of plant cell walls. Dolomite occurs as diagenetic microdolomite associated with the fibrous carbonate phase, as sparite replacements, and as void-filling cement. Maximum dolomite (50-59 wt.%) is in the top-of-seam coal-ball zone at the Sahara Mine, which is overlain by the marine Anna Shale. Coal-ball formation in the Herrin Coal began with the precipitation of fibrous high magnesium calcite. The trigonal prism morphology of the carbonate fibers suggests rapid precipitation from super-saturated, meteoric pore waters. Carbonate precipitation from marine waters is discounted on the basis of stratigraphic, paleobotanical, and stable isotopic evidence. Most non-fibrous carbonate is attributable to later diagenetic events, including void-fill replacements, recrystallization, and post-depositional fracture fills. Evidence suggests that CO2 degassing was important in coal-ball formation in the Herrin Coal, which mainly occurred sequentially upward with peat accumulation in the sites studied.

Mineralogy and Geochemistry of the Main Glauconite Bed in the Middle Eocene of Texas: Paleoenvironmental Implications for the Verdine Facies

PubMed Central

Harding, Sherie C.; Nash, Barbara P.; Petersen, Erich U.; Ekdale, A. A.; Bradbury, Christopher D.; Dyar, M. Darby

2014-01-01

The Main Glauconite Bed (MGB) is a pelleted greensand located at Stone City Bluff on the south bank of the Brazos River in Burleson County, Texas. It was deposited during the Middle Eocene regional transgression on the Texas Gulf Coastal Plain. Stratigraphically it lies in the upper Stone City Member, Crockett Formation, Claiborne Group. Its mineralogy and geochemistry were examined in detail, and verdine facies minerals, predominantly odinite, were identified. Few glauconitic minerals were found in the green pelleted sediments of the MGB. Without detailed mineralogical work, glaucony facies minerals and verdine facies minerals are easily mistaken for one another. Their distinction has value in assessing paleoenvironments. In this study, several analytical techniques were employed to assess the mineralogy. X-ray diffraction of oriented and un-oriented clay samples indicated a clay mixture dominated by 7 and 14Å diffraction peaks. Unit cell calculations from XRD data for MGB pellets match the odinite-1M data base. Electron microprobe analyses (EMPA) from the average of 31 data points from clay pellets accompanied with Mössbauer analyses were used to calculate the structural formula which is that of odinite: Fe3+ 0.89 Mg0.45 Al0.67 Fe2+ 0.30 Ti0.01 Mn0.01) Σ = 2.33 (Si1.77 Al0.23) O5.00 (OH)4.00. QEMSCAN (Quantitative Evaluation of Minerals by Scanning Electron Microscopy) data provided mineral maps of quantitative proportions of the constituent clays. The verdine facies is a clay mineral facies associated with shallow marine shelf and lagoonal environments at tropical latitudes with iron influx from nearby runoff. Its depositional environment is well documented in modern nearshore locations. Recognition of verdine facies clays as the dominant constituent of the MGB clay pellets, rather than glaucony facies clays, allows for a more precise assessment of paleoenvironmental conditions. PMID:24503875

Interactions of bioactive glass materials in the oral environment

NASA Astrophysics Data System (ADS)

Efflandt, Sarah Elizabeth

The aim of this research was to investigate bioactive glass materials for their use in dental restorations. Mechanical properties such as strength, toughness and wear resistance were considered initially, but the focus of this thesis was the biological properties such as reactions with saliva and interactions with natural dental tissues. Bioactive composite materials were created by incorporating bioactive glass and alumina powders into an aqueous suspension, slip casting, and infiltrating with resin. Microstructure, mechanical properties and wear resistance were evaluated. Mechanically, the composites are comparable to natural dental tissues and current dental materials with a strength of 206 +/- 18.7 MPa and a toughness of 1.74 +/- 0.08 MPa(m)1/2. Interfacial reactions were examined using bulk bioactive glasses. Disks were prepared from a melt, placed in saliva and incubated at 37°C. Surfaces were analyzed at 2, 5, 10, 21, and 42 days using scanning electron microscopy (SEM) and microdiffraction. Results showed changes at 2 days with apatite crystallization by 10 days. These glass disks were then secured against extracted human dentin and incubated in saliva for 21 or 42 days. Results from SEM, electron microprobe analysis (EMPA) and microdiffraction showed that dentin and bioactive glasses adhered in this in vitro environment due to attraction of collagen to bioactive glasses and growth of an interfacial apatite. After investigating these bulk glass responses, particulate bioactive glasses were placed in in vitro and in vivo set-ups for evaluation. Particles immersed in biologically buffered saliva showed crystallization of apatite at 3 days. These bioactive glass particles were placed in the molars of mini-pigs and left in vivo. After 30 days the bioactive paste was evaluated using SEM, EMPA and microdiffraction analyses. Results showed that the paste gained structural integrity and had chemical changes in vivo. These sets of experiments show that bioactive glasses have many mechanical and biological characteristics desirable for use in dental materials. Hopefully, the conclusions presented here will lead to further investigations toward their use in dentistry.

Experimental study of the mechanism and sequence of calcite-dolomite replacement

NASA Astrophysics Data System (ADS)

Moraila-Martinez, Teresita; Putnis, Christine V.; Putnis, Andrew

2015-04-01

For many years the formation, mechanism and environmental settings of dolomite formation have been under discussion, mainly because dolomite is commonly found in ancient rocks, whereas it is rarely present in modern sediments. The most favoured hypothesis is the 'dolomitization' of limestone by Mg-bearing aqueous solutions [1,2]. The existence of sharp limestone-dolomite contacts in natural rocks suggests that dolomitization involves a coupled dissolution-precipitation process. For a better understanding of the replacement mechanism of calcite by dolomite we performed hydrothermal experiments using Carrara marble cubes of 1.5 mm size, that reacted with 1M (Ca,Mg)Cl2 solutions with a Mg:Ca ratio of 3, at 200°C for different duration times (10, 20, 40, 50 and 58 days). After reaction, the product phases were characterized using Raman spectroscopy, electron microprobe analysis, and scanning electron microscopy. After reaction, the external morphology of the samples was preserved. Back-scattered images revealed two replacement end products: dolomite and magnesite. Grain boundaries of the samples were maintained. Shorter time duration experiments resulted in the replacement reaction occurring mainly along grain boundaries, whereas in longer duration time experiments more replacement was located in the core of the sample. In this type of reaction, grain boundaries are very important for the replacement to occur, acting as fluid pathways, allowing the infiltration of the solution further from the rock surface, enhancing fluid permeability within the sample and allowing further replacement reactions to occur. 1. Kaczmarek S.E., Sibley D.F. On the evolution of dolomite stoichiometry and cation order during high temperature synthesis experiments: An alternative model for geochemical evolution of natural dolomites. Sedimentary Geology. 240, 30-40 (2011). 2. Etschmann B., Brugger J., Pearce M.A., Ta C., Brautigan D., Jung M., Pring A. Grain boundaries as microreactors during reactive fluid flow: experimental dolomitization of a calcite marble. Contributions to Mineralogy and Petrology. 168:1045 (2014).

Trace-metal sources and their release from mine wastes: examples from humidity cell tests of hardrock mine waste and from Warrior Basin coal

USGS Publications Warehouse

Diehl, S.F.; Smith, Kathleen S.; Desborough, G.A.; White, W.W.; Lapakko, K.A.; Goldhaber, Martin B.; Fey, David L.

2003-01-01

To assess the potential impact of metal and acid contamination from mine-waste piles, it is important to identify the mineralogic source of trace metals and their mode of occurrence. Microscopic analysis of mine-waste samples from both hard-rock and coalmine waste samples demonstrate a microstructural control, as well as mineralogic control, on the source and release of trace metals into local water systems. The samples discussed herein show multiple periods of sulfide mineralization with varying concentrations of trace metals. In the first case study, two proprietary hard-rock mine-waste samples exposed to a series of humidity cell tests (which simulate intense chemical weathering conditions) generated acid and released trace metals. Some trace elements of interest were: arsenic (45-120 ppm), copper (60-320 ppm), and zinc (30-2,500 ppm). Untested and humidity cell-exposed samples were studied by X-ray diffraction, scanning electron microscope with energy dispersive X-ray (SEM/EDX), and electron microprobe analysis. Studies of one sample set revealed arsenic-bearing pyrite in early iron- and magnesium-rich carbonate-filled microveins, and iron-, copper-, arsenic-, antimony-bearing sulfides in later crosscutting silica-filled microveins. Post humidity cell tests indicated that the carbonate minerals were removed by leaching in the humidity cells, exposing pyrite to oxidative conditions. However, sulfides in the silica-filled veins were more protected. Therefore, the trace metals contained in the sulfides within the silica-filled microveins may be released to the surface and (or) ground water system more slowly over a greater time period. In the second case study, trace metal-rich pyrite-bearing coals from the Warrior Basin, Alabama were analyzed. Arsenic-bearing pyrite was observed in a late-stage pyrite phase in microfaults and microveins that crosscut earlier arsenic.

Magmatic (silicates/saline/sulfur-rich/CO2) immiscibility and zirconium and rare-earth element enrichment from alkaline magma chamber margins : Evidence from Ponza Island, Pontine Archipelago, Italy

USGS Publications Warehouse

Belkin, H.E.; de Vivo, B.; Lima, A.; Torok, K.

1996-01-01

Fluid inclusions were measured from a feldspathoid-bearing syenite xenolith entrained in trachyte from Ponza, one of the islands of the Pontine Archipelago, located in the Gulf of Gaeta, Italy. The feldspathoid-bearing syenite consists mainly of potassium feldspar, clinopyroxene, amphibole, biotite, titanite, manganoan magnetite, apatite with minor nosean, Na-rich feldspar, pyrrhotite, and rare cheralite. Baddeleyite and zirkelite occur associated with manganoan magnetite. Detailed electron-microprobe analysis reveals enrichments in REE, Y, Nb, U, Th as well as Cl and F in appropriate phases. Fluid inclusions observed in potassium feldspar are either silicate-melt or aqueous inclusions. The aqueous inclusions can be further classified as. (1) one-phase vapor, (2) two-phase (V + L) inclusions, vapor-rich inclusions with a small amount of CO2 in most cases; homogenization of the inclusions always occurred in the vapor phase between 359 and 424??C, salinities vary from 2.9 to 8.5 wt. % NaCl equivalent; and. (3) three-phase and multiphase inclusions (hypersaline/sulfur-rich aqueous inclusions sometimes with up to 8 or more solid phases). Daughter minerals dissolve on heating before vapor/liquid homogenization. Standardless quantitative scanning electron microscope X-ray fluorescence analysis has tentatively identified the following chloride and sulfate daughter crystals; halite, sylvite, glauberite. arcanite, anhydrite, and thenardite. Melting of the daughter crystals occurs between 459 and 536??C (54 to 65 wt. % NaCI equivalent) whereas total homogenization is between 640 and 755??C. The occurrence of silicate-melt inclusions and high-temperature, solute-rich aqueous inclusions suggests that the druse or miarolitic texture of the xenolith is late-stage magmatic. The xenolith from Ponza represents a portion of the peripheral magma chamber wall that has recorded the magmatic/hydrothermal transition and the passage of high solute fluids enriched in chlorides, sulfur, and incompatible elements.

Diagenesis of fossil coral skeletons: Correlation between trace elements, textures, and [sup 234]U/[sup 238]U

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

Bar-Matthews, M.; Wasserburg, G.J.; Chen, J.H.

1993-01-01

A comparative study of Pleistocene fossil coral skeletons and of modern coral skeletons was carried out using petrographic and trace element analyses on a suite of Pleistocene samples that had previously been studied from [sup 234]U, [sup 230]Th, and U-[sup 230]Th ages (Chen et al. 1991). Evidence of a range of diagenetic changes can be recognized by optical (OM) and scanning electron microscopy (SEM). Using an electron microprobe and SEM, concentrations of Na, S, Sr, and Mg were measured. No other trace elements were detected. Na, S, and Mg contents of the matrix, the fibrous micropores, and radiating needles aremore » highly variable and well correlated. High concentrations of Na, S, and Mg were found in modern living corals with lower concentrations in fossil corals and fibrous micropores, and the lowest value in the radiating needles. The reason for the correlations of Na, S, and Mg and crystal chemistry and the response to diagenesis of these trace elements is not understood. The average concentrations of Na, S, and Mg for each sample, when plotted against the whole coral initial [delta][sup 234]U, are generally correlated (Chen et al., 1991). As all these diagenetic changes involve the recystallization and deposition of aragonite, the authors infer that the geologic site of diagenesis both for forming the secondary aragonitic phases and for the enhancement of the [sup 234]U content in the fossil corals was the marine environment. It is possible that the textural and Na, S, and Mg trace element contents of fossil corals be used to ascertain the reliability of fossil coral skeletons for U-[sup 230]Th dating. The basic problem of identifying a priori unaltered coral skeletons for [sup 230]Th dating is not yet resolved. 64 refs., 16 figs., 5 tabs.« less

Chemistry of chromites from Arroio Grande Ophiolite (Dom Feliciano Belt, Brazil) and their possible connection with the Nama Group (Namibia)

NASA Astrophysics Data System (ADS)

Ramos, Rodrigo Chaves; Koester, Edinei; Porcher, Carla Cristine

2017-12-01

The present paper shows a mineral chemistry study in chromites found in serpentine-talc schists of the Arroio Grande Ophiolite, located in the southeastern Dom Feliciano Belt, near the Brazil/Uruguay border. Using electron microscope scanning and electron microprobe techniques, this study found a supra-subduction zone signature in the chromites, together with evidence of metasomatism. It corroborates previous hypothesis that suggested a supra-subduction zone origin for the protoliths of the Arroio Grande meta-igneous rocks and a metasomatic origin for the chromite-bearing magnesian schists. The studied chromites present high Cr# (0.65-0.77) and Fe2+# (0.88-0.95), low MgO (0.85-2.47 wt%) and TiO2 (0.01-0.19 wt%) and anomalous high concentration of ZnO (up to 1.97 wt%). The results were compared with chemical data from detrital chromites from the Schwarzrand and Fish River Subgroups of the Nama Group (Namibia), demonstrating that they are compositionally similar with those found in the latter. These chromites, in turn, are believed to have been derived from the oceanic Marmora Terrane (Gariep Belt) in the west (present-day coordinates). Taking into consideration that oceanic metamafites from both the latter and the Arroio Grande Ophiolite share common bulk-rock geochemical features (in this paper interpreted as fragments of the same paleo-ocean floor - the Marmora back-arc basin), it is possible to raise the hypothesis that detrital material derived from the studied ophiolite might also be found in Nama Group. It is reinforced by the fact that sediments (related to the Pelotas-Aiguá Batholith granitoids) derived from the easternmost Dom Feliciano Belt, i.e. the region where Arroio Grande Ophiolite is located, is found in both Schwarzrand and Fish River Subgroups. Thus, we suggest that Arroio Grande Ophiolite detrital sediments might also have contributed to the Nama Basin infilling during Late Ediacaran-Lower Cambrian.

Interpreting U-Pb data from primary and secondary features in lunar zircon

NASA Astrophysics Data System (ADS)

Grange, M. L.; Pidgeon, R. T.; Nemchin, A. A.; Timms, N. E.; Meyer, C.

2013-01-01

In this paper, we describe primary and secondary microstructures and textural characteristics found in lunar zircon and discuss the relationships between these features and the zircon U-Pb isotopic systems and the significance of these features for understanding lunar processes. Lunar zircons can be classified according to: (i) textural relationships between zircon and surrounding minerals in the host breccias, (ii) the internal microstructures of the zircon grains as identified by optical microscopy, cathodoluminescence (CL) imaging and electron backscattered diffraction (EBSD) mapping and (iii) results of in situ ion microprobe analyses of the Th-U-Pb isotopic systems. Primary zircon can occur as part of a cogenetic mineral assemblage (lithic clast) or as an individual mineral clast and is unzoned, or has sector and/or oscillatory zoning. The age of primary zircon is obtained when multiple ion microprobe analyses across the polished surface of the grain give reproducible and essentially concordant data. A secondary set of microstructures, superimposed on primary zircon, include localised recrystallised domains, localised amorphous domains, crystal-plastic deformation, planar deformation features and fractures, and are associated with impact processes. The first two secondary microstructures often yield internally consistent and close to concordant U-Pb ages that we interpret as dating impact events. Others secondary microstructures such as planar deformation features, crystal-plastic deformation and micro-fractures can provide channels for Pb diffusion and result in partial resetting of the U-Pb isotopic systems.

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.

A new apparatus for electron tomography in the scanning electron microscope

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

Morandi, V., E-mail: morandi@bo.imm.cnr.it; Maccagnani, P.; Masini, L.

2015-06-23

The three-dimensional reconstruction of a microscopic specimen has been obtained by applying the tomographic algorithm to a set of images acquired in a Scanning Electron Microscope. This result was achieved starting from a series of projections obtained by stepwise rotating the sample under the beam raster. The Scanning Electron Microscope was operated in the scanning-transmission imaging mode, where the intensity of the transmitted electron beam is a monotonic function of the local mass-density and thickness of the specimen. The detection strategy has been implemented and tailored in order to maintain the projection requirement over the large tilt range, as requiredmore » by the tomographic workflow. A Si-based electron detector and an eucentric-rotation specimen holder have been specifically developed for the purpose.« less

Subsurface examination of a foliar biofilm using scanning electron- and focused-ion-beam microscopy

USDA-ARS?s Scientific Manuscript database

The dual beam scanning electron microscope, equipped with both a focused ion- and scanning electron- beam (FIB SEM) is a novel tool for the exploration of the subsurface structure of biological tissues. The FIB is capable of removing small cross sections to view the subsurface features and may be s...

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.

Trace element analysis by EPMA in geosciences: detection limit, precision and accuracy

NASA Astrophysics Data System (ADS)

Batanova, V. G.; Sobolev, A. V.; Magnin, V.

2018-01-01

Use of the electron probe microanalyser (EPMA) for trace element analysis has increased over the last decade, mainly because of improved stability of spectrometers and the electron column when operated at high probe current; development of new large-area crystal monochromators and ultra-high count rate spectrometers; full integration of energy-dispersive / wavelength-dispersive X-ray spectrometry (EDS/WDS) signals; and the development of powerful software packages. For phases that are stable under a dense electron beam, the detection limit and precision can be decreased to the ppm level by using high acceleration voltage and beam current combined with long counting time. Data on 10 elements (Na, Al, P, Ca, Ti, Cr, Mn, Co, Ni, Zn) in olivine obtained on a JEOL JXA-8230 microprobe with tungsten filament show that the detection limit decreases proportionally to the square root of counting time and probe current. For all elements equal or heavier than phosphorus (Z = 15), the detection limit decreases with increasing accelerating voltage. The analytical precision for minor and trace elements analysed in olivine at 25 kV accelerating voltage and 900 nA beam current is 4 - 18 ppm (2 standard deviations of repeated measurements of the olivine reference sample) and is similar to the detection limit of corresponding elements. To analyse trace elements accurately requires careful estimation of background, and consideration of sample damage under the beam and secondary fluorescence from phase boundaries. The development and use of matrix reference samples with well-characterised trace elements of interest is important for monitoring and improving of the accuracy. An evaluation of the accuracy of trace element analyses in olivine has been made by comparing EPMA data for new reference samples with data obtained by different in-situ and bulk analytical methods in six different laboratories worldwide. For all elements, the measured concentrations in the olivine reference sample were found to be identical (within internal precision) to reference values, suggesting that achieved precision and accuracy are similar. The spatial resolution of EPMA in a silicate matrix, even at very extreme conditions (accelerating voltage 25 kV), does not exceed 7 - 8 μm and thus is still better than laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) or secondary ion mass spectrometry (SIMS) of similar precision. These make the electron microprobe an indispensable method with applications in experimental petrology, geochemistry and cosmochemistry.

Spatial Resolution in Scanning Electron Microscopy and Scanning Transmission Electron Microscopy Without a Specimen Vacuum Chamber.

PubMed

Nguyen, Kayla X; Holtz, Megan E; Richmond-Decker, Justin; Muller, David A

2016-08-01

A long-standing goal of electron microscopy has been the high-resolution characterization of specimens in their native environment. However, electron optics require high vacuum to maintain an unscattered and focused probe, a challenge for specimens requiring atmospheric or liquid environments. Here, we use an electron-transparent window at the base of a scanning electron microscope's objective lens to separate column vacuum from the specimen, enabling imaging under ambient conditions, without a specimen vacuum chamber. We demonstrate in-air imaging of specimens at nanoscale resolution using backscattered scanning electron microscopy (airSEM) and scanning transmission electron microscopy. We explore resolution and contrast using Monte Carlo simulations and analytical models. We find that nanometer-scale resolution can be obtained at gas path lengths up to 400 μm, although contrast drops with increasing gas path length. As the electron-transparent window scatters considerably more than gas at our operating conditions, we observe that the densities and thicknesses of the electron-transparent window are the dominant limiting factors for image contrast at lower operating voltages. By enabling a variety of detector configurations, the airSEM is applicable to a wide range of environmental experiments including the imaging of hydrated biological specimens and in situ chemical and electrochemical processes.

Spatial Resolution in Scanning Electron Microscopy and Scanning Transmission Electron Microscopy Without a Specimen Vacuum Chamber

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

Nguyen, Kayla X.; Holtz, Megan E.; Richmond-Decker, Justin

2016-07-25

Abstract A long-standing goal of electron microscopy has been the high-resolution characterization of specimens in their native environment. However, electron optics require high vacuum to maintain an unscattered and focused probe, a challenge for specimens requiring atmospheric or liquid environments. Here, we use an electron-transparent window at the base of a scanning electron microscope’s objective lens to separate column vacuum from the specimen, enabling imaging under ambient conditions, without a specimen vacuum chamber. We demonstrate in-air imaging of specimens at nanoscale resolution using backscattered scanning electron microscopy (airSEM) and scanning transmission electron microscopy. We explore resolution and contrast using Montemore » Carlo simulations and analytical models. We find that nanometer-scale resolution can be obtained at gas path lengths up to 400μm, although contrast drops with increasing gas path length. As the electron-transparent window scatters considerably more than gas at our operating conditions, we observe that the densities and thicknesses of the electron-transparent window are the dominant limiting factors for image contrast at lower operating voltages. By enabling a variety of detector configurations, the airSEM is applicable to a wide range of environmental experiments including the imaging of hydrated biological specimens andin situchemical and electrochemical processes.« less

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.

A scanning electron microscopy study of the macro-crystalline structure of 2-(2,4-dinitrobenzyl) pyridine

NASA Technical Reports Server (NTRS)

Ware, Jacqueline; Hammond, Ernest C., Jr.

1989-01-01

The compound, 2-(2,4-dinitrobenzyl) pyridine, was synthesized in the laboratory; an introductory level electron microscopy study of the macro-crystalline structure was conducted using the scanning electron microscope (SEM). The structure of these crystals was compared with the macrostructure of the crystal of 2-(2,4-dinitrobenzyl) pyridinium bromide, the hydrobromic salt of the compound which was also synthesized in the laboratory. A scanning electron microscopy crystal study was combined with a study of the principle of the electron microscope.

U-10Mo Sample Preparation and Examination using Optical and Scanning Electron Microscopy

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

Prabhakaran, Ramprashad; Joshi, Vineet V.; Rhodes, Mark A.

2016-10-01

The purpose of this document is to provide guidelines to prepare specimens of uranium alloyed with 10 weight percent molybdenum (U-10Mo) for optical metallography and scanning electron microscopy. This document also provides instructions to set up an optical microscope and a scanning electron microscope to analyze U-10Mo specimens and to obtain the required information.

U-10Mo Sample Preparation and Examination using Optical and Scanning Electron Microscopy

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

Prabhakaran, Ramprashad; Joshi, Vineet V.; Rhodes, Mark A.

2016-03-30

The purpose of this document is to provide guidelines to prepare specimens of uranium alloyed with 10 weight percent molybdenum (U-10Mo) for optical metallography and scanning electron microscopy. This document also provides instructions to set up an optical microscope and a scanning electron microscope to analyze U-10Mo specimens and to obtain the required information.

Time scales of porphyry Cu deposit formation: insights from titanium diffusion in quartz

USGS Publications Warehouse

Mercer, Celestine N.; Reed, Mark H.; Mercer, Cameron M.

2015-01-01

Porphyry dikes and hydrothermal veins from the porphyry Cu-Mo deposit at Butte, Montana, contain multiple generations of quartz that are distinct in scanning electron microscope-cathodoluminescence (SEM-CL) images and in Ti concentrations. A comparison of microprobe trace element profiles and maps to SEM-CL images shows that the concentration of Ti in quartz correlates positively with CL brightness but Al, K, and Fe do not. After calibrating CL brightness in relation to Ti concentration, we use the brightness gradient between different quartz generations as a proxy for Ti gradients that we model to determine time scales of quartz formation and cooling. Model results indicate that time scales of porphyry magma residence are ~1,000s of years and time scales from porphyry quartz phenocryst rim formation to porphyry dike injection and cooling are ~10s of years. Time scales for the formation and cooling of various generations of hydrothermal vein quartz range from 10s to 10,000s of years. These time scales are considerably shorter than the ~0.6 m.y. overall time frame for each porphyry-style mineralization pulse determined from isotopic studies at Butte, Montana. Simple heat conduction models provide a temporal reference point to compare chemical diffusion time scales, and we find that they support short dike and vein formation time scales. We interpret these relatively short time scales to indicate that the Butte porphyry deposit formed by short-lived episodes of hydrofracturing, dike injection, and vein formation, each with discrete thermal pulses, which repeated over the ~3 m.y. generation of the deposit.

Vivianite formation and distribution in Lake Baikal sediments

NASA Astrophysics Data System (ADS)

Fagel, N.; Alleman, L. Y.; Granina, L.; Hatert, F.; Thamo-Bozso, E.; Cloots, R.; André, L.

2005-04-01

In an effort to better understand vivianite formation processes, four Lake Baikal sediment cores spanning two to four interglacial stages in the northern, central and southern basins and under various biogeochemical environments are scrutinized. The vivianite-rich layers were detected by anomalous P-enrichments in bulk geochemistry and visually by observations on X-radiographs. The millimetric concretions of vivianite were isolated by sieving and analysed by X-ray diffraction, scanning electron microscope (SEM), microprobe, infrared spectroscopy, inductively coupled plasma atomic emission spectrometry and mass spectrometry (ICP-AES, ICP-MS). All the vivianites display similar morphological, mineralogical and geochemical signature, suggesting a common diagenetic origin. Their geochemical signature is sensitive to secondary alteration where vivianite concretions are gradually transformed from the rim to the center into an amorphous santabarbaraite phase with a decreasing Mn content. We analysed the spatial and temporal distribution of the concretions in order to determine the primary parameters controlling the vivianite formation, e.g., lithology, sedimentation rates, and porewater chemistry. We conclude that vivianite formation in Lake Baikal is mainly controlled by porewater chemistry and sedimentation rates, and it is not a proxy for lacustrine paleoproductivity. Vivianite accumulation is not restricted to areas of slow sedimentation rates (e.g., Academician and Continent ridges). At the site of relatively fast sedimentation rate, i.e., the Posolsky Bank near the Selenga Delta, vivianite production may be more or less related to the Selenga River inputs. It could be also indirectly related to the past intensive methane escapes from the sediments. While reflecting an early diagenetic signal, the source of P and Fe porewater for vivianites genesis is still unclear.

Electrostatic solitary waves generated by beam injection in LAPD

NASA Astrophysics Data System (ADS)

Chen, L.; Gekelman, W. N.; Lefebvre, B.; Kintner, P. M.; Pickett, J. S.; Pribyl, P.; Vincena, S. T.

2011-12-01

Spacecraft data have revealed that electrostatic solitary waves are ubiquitous in non-equilibrium collisionless space plasmas. These solitary waves are often the main constituents of the observed electrostatic turbulence. The ubiquitous presence of these solitary waves in space motivated laboratory studies on their generation and evolution in the Large Plasma Device (LAPD) at UCLA. In order to observe these structures, microprobes with scale sizes of order of the Debye length (30 microns) had to be built using Mems technology. A suprathermal electron beam was injected into the afterglow plasma, and solitary waves as well as nonlinear wave packets were measured. The solitary waves are interpreted as BGK electron holes based on their width, amplitude, and velocity characteristics. The ensuing turbulence, including the solitary waves and wave packets, exhibits a band dispersion relation with its central line consistent with the electrostatic whistler mode. One surprise brought by the laboratory experiments is that the electron holes were not generated through resonant two-stream instabilities, but likely through an instability due to parallel currents. The characteristics of the LAPD electron holes and those observed in space will be compared to motivate further theoretical, simulation, and experimental work.

Signatures in Martian Volatiles and the Magma Sources of NC Meteorites

NASA Technical Reports Server (NTRS)

Marti, K.; Mathew, K. J.

2004-01-01

We report nitrogen and xenon isotopic signatures in Yamato nakhlites and use the data to assess properties of the magma source of NC meteorites in planet Mars. The Chassigny meteorite was investigated by Floran et al, who classified it as a cumulate dunite with hydrous amphibole-bearing melt inclusions with no preferred orientation of the olivines. Their inferred composition of the parent magma, which was based on electron microprobe analyses, has been questioned. The trace and minor elements in minerals were analyzed in nakhlites and in Chassigny and the authors conclude that nakhlites may represent samples from different horizons of the same lithologic unit, but that Chassigny was not co-magmatic with the nakhlites.

The parent magma of the Nakhla (SNC) meteorite: Reconciliation of composition estimates from magmatic inclusions and element partitioning

NASA Technical Reports Server (NTRS)

Treiman, A. H.

1993-01-01

The composition of the parent magma of the Nakhla meteorite was difficult to determine, because it is accumulate rock, enriched in olivine and augite relative to a basalt magma. A parent magma composition is estimated from electron microprobe area analyses of magmatic inclusions in olivine. This composition is consistent with an independent estimate based on the same inclusions, and with chemical equilibria with the cores of Nakhla's augites. This composition reconciles most of the previous estimates of Nakhla's magma composition, and obviates the need for complex magmatic processes. Inconsistency between this composition and those calculated previously suggests that magma flowed through and crystallized into Nakhla as it cooled.

Rapid Classification of Ordinary Chondrites Using Raman Spectroscopy

NASA Technical Reports Server (NTRS)

Fries, M.; Welzenbach, L.

2014-01-01

Classification of ordinary chondrites is typically done through measurements of the composition of olivine and pyroxenes. Historically, this measurement has usually been performed via electron microprobe, oil immersion or other methods which can be costly through lost sample material during thin section preparation. Raman microscopy can perform the same measurements but considerably faster and with much less sample preparation allowing for faster classification. Raman spectroscopy can facilitate more rapid classification of large amounts of chondrites such as those retrieved from North Africa and potentially Antarctica, are present in large collections, or are submitted to a curation facility by the public. With development, this approach may provide a completely automated classification method of all chondrite types.

Paired lunar meteorites MAC88104 and MAC88105 - A new 'FAN' of lunar petrology

NASA Astrophysics Data System (ADS)

Neal, Clive R.; Taylor, Lawrence A.; Lui, Yun-Gang; Schmitt, Roman A.

1991-11-01

To determine the chemical characteristics of the MAC88104/5 meteorite six thin sections and three bulk samples were analyzed by electron microprobe and instrumental neutron activation. It is concluded that this meteorite is dominated by lithologies of the ferroan anorthosite suite and contains abundant granulitized highland clasts, devitrified glass beads of impact origin, and two small clasts of basaltic origin. It is suggested that one of these basaltic clasts, clast E, is mesostasis material, and clast G is similar to the very low-Ti or low-Ti/high-alumina mare basalts. Impact melt clasts MAC88105, 69, and 72 have major and trace element compositions similar to the bulk meteorite.

Surface aspects of pitting and stress corrosion cracking

NASA Technical Reports Server (NTRS)

Truhan, J. S., Jr.; Hehemann, R. F.

1977-01-01

The pitting and stress corrosion cracking of a stable austenitic stainless steel in aqueous chloride environments were investigated using a secondary ion mass spectrometer as the primary experimental technique. The surface concentration of hydrogen, oxygen, the hydroxide, and chloride ion, magnesium or sodium, chromium and nickel were measured as a function of potential in both aqueous sodium chloride and magnesium chloride environments at room temperature and boiling temperatures. It was found that, under anodic conditions, a sharp increase in the chloride concentration was observed to occur for all environmental conditions. The increase may be associated with the formation of an iron chloride complex. Higher localized chloride concentrations at pits and cracks were also detected with an electron microprobe.

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.

High-intensity positron microprobe at the Thomas Jefferson National Accelerator Facility

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

Golge, S., E-mail: serkan.golge@nasa.gov; Vlahovic, B.; Wojtsekhowski, B.

We present a conceptual design for a novel continuous wave electron-linac based high-intensity high-brightness slow-positron production source with a projected intensity on the order of 10{sup 10 }e{sup +}/s. Reaching this intensity in our design relies on the transport of positrons (T{sub +} below 600 keV) from the electron-positron pair production converter target to a low-radiation and low-temperature area for moderation in a high-efficiency cryogenic rare gas moderator, solid Ne. This design progressed through Monte Carlo optimizations of: electron/positron beam energies and converter target thickness, transport of the e{sup +} beam from the converter to the moderator, extraction of the e{sup +}more » beam from the magnetic channel, a synchronized raster system, and moderator efficiency calculations. For the extraction of e{sup +} from the magnetic channel, a magnetic field terminator plug prototype has been built and experimental results on the effectiveness of the prototype are presented. The dissipation of the heat away from the converter target and radiation protection measures are also discussed.« less

Probing molecular dynamics in solution with x-ray valence-to-core spectroscopy

NASA Astrophysics Data System (ADS)

Doumy, Gilles; March, Anne Marie; Tu, Ming-Feng; Al Haddad, Andre; Southworth, Stephen; Young, Linda; Walko, Donald; Bostedt, Christoph

2017-04-01

Hard X-ray spectroscopies are powerful tools for probing the electronic and geometric structure of molecules in complex or disordered systems and have been particularly useful for studying molecules in the solution phase. They are element specific, sensitive to the electronic structure and the local arrangements of surrounding atoms of the element being selectively probed. When combined in a pump-probe scheme with ultrafast lasers, X-ray spectroscopies can be used to track the evolution of structural changes that occur after photoexcitation. Efficient use of hard x-ray radiation coming from high brilliance synchrotrons and upcoming high repetition rate X-ray Free Electron Lasers requires MHz repetition rate lasers and data acquisition systems. High information content Valence-to-Core x-ray emission is directly sensitive to the molecular orbitals involved in photochemistry. We report on recent progress towards fully enabling this photon-hungry technique for the study of time-resolved molecular dynamics, including efficient detection and use of polychromatic x-ray micro-probe at the Advanced Photon Source. Work was supported by the U.S. Department of Energy, Office of Science, Chemical Sciences, Geosciences, and Biosciences Division.

Simultaneous assessment of phase chemistry, phase abundance and bulk chemistry with statistical electron probe micro-analyses: Application to cement clinkers

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

Wilson, William; Krakowiak, Konrad J.; Ulm, Franz-Josef, E-mail: ulm@mit.edu

2014-01-15

According to recent developments in cement clinker engineering, the optimization of chemical substitutions in the main clinker phases offers a promising approach to improve both reactivity and grindability of clinkers. Thus, monitoring the chemistry of the phases may become part of the quality control at the cement plants, along with the usual measurements of the abundance of the mineralogical phases (quantitative X-ray diffraction) and the bulk chemistry (X-ray fluorescence). This paper presents a new method to assess these three complementary quantities with a single experiment. The method is based on electron microprobe spot analyses, performed over a grid located onmore » a representative surface of the sample and interpreted with advanced statistical tools. This paper describes the method and the experimental program performed on industrial clinkers to establish the accuracy in comparison to conventional methods. -- Highlights: •A new method of clinker characterization •Combination of electron probe technique with cluster analysis •Simultaneous assessment of phase abundance, composition and bulk chemistry •Experimental validation performed on industrial clinkers.« less

Filling the holes in the CaFe4As3 structure: Synthesis and magnetism of CaCo5As3

NASA Astrophysics Data System (ADS)

Rosa, P. F. S.; Scott, B. L.; Ronning, F.; Bauer, E. D.; Thompson, J. D.

2017-07-01

Here, we investigate single crystals of CaCo5As3 by means of single-crystal x-ray diffraction, microprobe, magnetic susceptibility, heat capacity, and pressure-dependent transport measurements. CaCo5As3 shares the same structure of CaFe4As3 with an additional Co atom filling a lattice vacancy and undergoes a magnetic transition at TM=16 K associated with a frustrated magnetic order. CaCo5As3 displays metallic behavior and its Sommerfeld coefficient (γ =70 mJ/mol K2) indicates a moderate enhancement of electron-electron correlations. Transport data under pressures to 2.5 GPa reveal a suppression of TM at a rate of -0.008 K/GPa. First-principles electronic structure calculations show a complex three-dimensional band structure and magnetic moments that depend on the local environment at each Co site. Our results are compared with previous data on CaFe4As3 and provide a scenario for a magnetically frustrated ground state in this family of compounds.

High-intensity positron microprobe at Jefferson Lab

DOE PAGES

Golge, Serkan; Vlahovic, Branislav; Wojtsekhowski, Bogdan B.

2014-06-19

We present a conceptual design for a novel continuous wave electron-linac based high-intensity slow-positron production source with a projected intensity on the order of 10 10 e +/s. Reaching this intensity in our design relies on the transport of positrons (T + below 600 keV) from the electron-positron pair production converter target to a low-radiation and low-temperature area for moderation in a high-efficiency cryogenic rare gas moderator, solid Ne. The performance of the integrated beamline has been verified through computational studies. The computational results include Monte Carlo calculations of the optimized electron/positron beam energies, converter target thickness, synchronized raster system,more » transport of the beam from the converter target to the moderator, extraction of the beam from the channel, and moderation efficiency calculations. For the extraction of positrons from the magnetic channel a magnetic field terminator plug prototype has been built and experimental data on the effectiveness of this prototype are presented. The dissipation of the heat away from the converter target and radiation protection measures are also discussed.« less

Correcting nonlinear drift distortion of scanning probe and scanning transmission electron microscopies from image pairs with orthogonal scan directions

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

Ophus, Colin; Ciston, Jim; Nelson, Chris T.

Unwanted motion of the probe with respect to the sample is a ubiquitous problem in scanning probe and scanning transmission electron microscopies, causing both linear and nonlinear artifacts in experimental images. We have designed a procedure to correct these artifacts by using orthogonal scan pairs to align each measurement line-by-line along the slow scan direction, by fitting contrast variation along the lines. We demonstrate the accuracy of our algorithm on both synthetic and experimental data and provide an implementation of our method.

Correcting nonlinear drift distortion of scanning probe and scanning transmission electron microscopies from image pairs with orthogonal scan directions

DOE PAGES

Ophus, Colin; Ciston, Jim; Nelson, Chris T.

2015-12-10

Unwanted motion of the probe with respect to the sample is a ubiquitous problem in scanning probe and scanning transmission electron microscopies, causing both linear and nonlinear artifacts in experimental images. We have designed a procedure to correct these artifacts by using orthogonal scan pairs to align each measurement line-by-line along the slow scan direction, by fitting contrast variation along the lines. We demonstrate the accuracy of our algorithm on both synthetic and experimental data and provide an implementation of our method.

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

Raman microprobe analysis of single ramie fiber during mercerization

Treesearch

Akira Isogai; Umesh P. Agarwal; Rajai H. Atalla

2003-01-01

The Raman microprobe technique was applied to structural analysis of single ramie fibers during mercerization. Polarized laser beam was irradiated on a ramie fiber in 0-30 % NaOD/D2O with the electric vector at 0 or 90° to the fiber axis, and Raman spectra thus obtained were studied in relation to the concentration of NaOD in D2O. Conversion of -OH to -OD in ramie...

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

High-resolution, high-throughput imaging with a multibeam scanning electron microscope

PubMed Central

EBERLE, AL; MIKULA, S; SCHALEK, R; LICHTMAN, J; TATE, ML KNOTHE; ZEIDLER, D

2015-01-01

Electron–electron interactions and detector bandwidth limit the maximal imaging speed of single-beam scanning electron microscopes. We use multiple electron beams in a single column and detect secondary electrons in parallel to increase the imaging speed by close to two orders of magnitude and demonstrate imaging for a variety of samples ranging from biological brain tissue to semiconductor wafers. Lay Description The composition of our world and our bodies on the very small scale has always fascinated people, making them search for ways to make this visible to the human eye. Where light microscopes reach their resolution limit at a certain magnification, electron microscopes can go beyond. But their capability of visualizing extremely small features comes at the cost of a very small field of view. Some of the questions researchers seek to answer today deal with the ultrafine structure of brains, bones or computer chips. Capturing these objects with electron microscopes takes a lot of time – maybe even exceeding the time span of a human being – or new tools that do the job much faster. A new type of scanning electron microscope scans with 61 electron beams in parallel, acquiring 61 adjacent images of the sample at the same time a conventional scanning electron microscope captures one of these images. In principle, the multibeam scanning electron microscope’s field of view is 61 times larger and therefore coverage of the sample surface can be accomplished in less time. This enables researchers to think about large-scale projects, for example in the rather new field of connectomics. A very good introduction to imaging a brain at nanometre resolution can be found within course material from Harvard University on http://www.mcb80x.org/# as featured media entitled ‘connectomics’. PMID:25627873

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

The solubility and site preference of Fe{sup 3+} in Li{sub 7−3x}Fe{sub x}La{sub 3}Zr{sub 2}O{sub 12} garnets

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

Rettenwander, D., E-mail: daniel.rettenwander@sbg.ac.at; Geiger, C.A.; Tribus, M.

2015-10-15

A series of Fe{sup 3+}-bearing Li{sub 7}La{sub 3}Zr{sub 2}O{sub 12} (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 {sup 57}Fe Mössbauer spectroscopy. A maximum of about 0.25 Fe{sup 3+} pfu could be incorporated in Li{sub 7−3x}Fe{sub x}La{sub 3}Zr{sub 2}O{sub 12} garnet solid solutions. At Fe{sup 3+} 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 withmore » starting materials having intended Fe{sup 3+} contents lower than 0.52 Fe{sup 3+} pfu. Back-scattered electron images made with an electron microprobe also showed no phase other than garnet for these compositions. The lattice parameter, a{sub 0}, for all solid-solution garnets is similar with a value of a{sub 0}≈12.98 Å regardless of the amount of Fe{sup 3+}. {sup 57}Fe Mössbauer spectroscopic measurements indicate the presence of poorly- or nano-crystalline FeLaO{sub 3} in syntheses with Fe{sup 3+} contents greater than 0.16 Fe{sup 3+} pfu. The composition of different phase pure Li{sub 7−3x}Fe{sub x}La{sub 3}Zr{sub 2}O{sub 12} garnets, as determined by electron microprobe (Fe, La, Zr) and ICP-OES (Li) measurements, give Li{sub 6.89}Fe{sub 0.03}La{sub 3.05}Zr{sub 2.01}O{sub 12}, Li{sub 6.66}Fe{sub 0.06}La{sub 3.06}Zr{sub 2.01}O{sub 12}, Li{sub 6.54}Fe{sub 0.12}La{sub 3.01}Zr{sub 1.98}O{sub 12}, and Li{sub 6.19}Fe{sub 0.19}La{sub 3.02}Zr{sub 2.04}O{sub 12}. The {sup 57}Fe Mössbauer spectrum of cubic Li{sub 6.54}Fe{sub 0.12}La{sub 3.01}Zr{sub 1.98}O{sub 12} garnet indicates that most Fe{sup 3+} occurs at the special crystallographic 24d position, which is the standard tetrahedrally coordinated site in garnet. Fe{sup 3+} in smaller amounts occurs at a general 96h site, which is only present for certain Li-oxide garnets, and in Li{sub 6.54}Fe{sub 0.12}La{sub 3.01}Zr{sub 1.98}O{sub 12} this Fe{sup 3+} has a distorted 4-fold coordination. - Graphical abstract: Cubic nominally Li{sub 7}La{sub 3}Zr{sub 2}O{sub 12} (LLZO) garnet is a promising candidate to be used as a solid electrolyte in Li-ion batteries. A series of Fe{sup 3+}-bearing LLZO garnets was synthesized and characterized compositionally and structurally. {sup 57}Mössbauer measurements were made to determine where Fe is incorporated in the crystal structure. X-ray diffraction, electron microprobe, ICP-OES and {sup 57}Mössbauer measurements are needed to obtain a full description of the synthetic products, some of which contain small amounts of nano- or poorly crystalline FeLaO{sub 3}. - Highlights: • A series of Fe{sup 3+}-bearing Li{sub 7}La{sub 3}Zr{sub 2}O{sub 12} (LLZO) garnets was synthesized and characterized compositionally and structurally. • {sup 57}Mössbauer measurements were made to determine where Fe is incorporated in the crystal structure. • Most Fe{sup 3+} substitutes for Li{sup +} in LLZO at the 24d and 96h sites in the cubic phase (Ia-3d). • No more than about 0.25 Fe{sup 3+} pfu can be incorporated into the LLZO garnet structure. • X-ray powder diffractions measurements indicate the presence of both cubic and tetragonal garnets phases in some syntheses. • The probable presence of small amounts of poorly or nano-crystalline FeLaO3 can only be identified by Mössbauer spectroscopy.« less

High-resolution scanning precession electron diffraction: Alignment and spatial resolution.

PubMed

Barnard, Jonathan S; Johnstone, Duncan N; Midgley, Paul A

2017-03-01

Methods are presented for aligning the pivot point of a precessing electron probe in the scanning transmission electron microscope (STEM) and for assessing the spatial resolution in scanning precession electron diffraction (SPED) experiments. The alignment procedure is performed entirely in diffraction mode, minimising probe wander within the bright-field (BF) convergent beam electron diffraction (CBED) disk and is used to obtain high spatial resolution SPED maps. Through analysis of the power spectra of virtual bright-field images extracted from the SPED data, the precession-induced blur was measured as a function of precession angle. At low precession angles, SPED spatial resolution was limited by electronic noise in the scan coils; whereas at high precession angles SPED spatial resolution was limited by tilt-induced two-fold astigmatism caused by the positive spherical aberration of the probe-forming lens. Copyright © 2016 Elsevier B.V. All rights reserved.

The application of scanning electron microscopy to fractography

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

Brooks, C.R.; McGill, B.L.

1994-10-01

Many failures involve fracture, and determination of the fracture process is a key factor in understanding the failure. This is frequently accomplished by characterizing the topography of the fracture surface. Scanning electron microscopy has a prominent role in fractography due to three features of the scanning electron microscope (SEM): high resolution, great depth of field, and the ability to obtain chemical information via analysis of the X-rays generated by the electrons. A qualitative treatment is presented of the interaction of electrons with a sample and the effect of the SEM operating parameters on image formation, quality, and X-ray analysis. Fractographsmore » are presented to illustrate these features of scanning electron microscopy and to illustrate the limitations and precautions in obtaining fractographs and x-ray analyses. The review is concluded with examples of fracture surface features of metallic, ceramic, and polymeric materials.« less

On the Progress of Scanning Transmission Electron Microscopy (STEM) Imaging in a Scanning Electron Microscope.

PubMed

Sun, Cheng; Müller, Erich; Meffert, Matthias; Gerthsen, Dagmar

2018-04-01

Transmission electron microscopy (TEM) with low-energy electrons has been recognized as an important addition to the family of electron microscopies as it may avoid knock-on damage and increase the contrast of weakly scattering objects. Scanning electron microscopes (SEMs) are well suited for low-energy electron microscopy with maximum electron energies of 30 keV, but they are mainly used for topography imaging of bulk samples. Implementation of a scanning transmission electron microscopy (STEM) detector and a charge-coupled-device camera for the acquisition of on-axis transmission electron diffraction (TED) patterns, in combination with recent resolution improvements, make SEMs highly interesting for structure analysis of some electron-transparent specimens which are traditionally investigated by TEM. A new aspect is correlative SEM, STEM, and TED imaging from the same specimen region in a SEM which leads to a wealth of information. Simultaneous image acquisition gives information on surface topography, inner structure including crystal defects and qualitative material contrast. Lattice-fringe resolution is obtained in bright-field STEM imaging. The benefits of correlative SEM/STEM/TED imaging in a SEM are exemplified by structure analyses from representative sample classes such as nanoparticulates and bulk materials.

Imaging of Norway spruce early somatic embryos with the ESEM, Cryo-SEM and laser scanning microscope.

PubMed

Neděla, Vilém; Hřib, Jiří; Havel, Ladislav; Hudec, Jiří; Runštuk, Jiří

2016-05-01

This article describes the surface structure of Norway spruce early somatic embryos (ESEs) as a typical culture with asynchronous development. The microstructure of extracellular matrix covering ESEs were observed using the environmental scanning electron microscope as a primary tool and using the scanning electron microscope with cryo attachment and laser electron microscope as a complementary tool allowing our results to be proven independently. The fresh samples were observed in conditions of the air environment of the environmental scanning electron microscope (ESEM) with the pressure from 550Pa to 690Pa and the low temperature of the sample from -18°C to -22°C. The samples were studied using two different types of detector to allow studying either the thin surface structure or material composition. The scanning electron microscope with cryo attachment was used for imaging frozen extracellular matrix microstructure with higher resolution. The combination of both electron microscopy methods was suitable for observation of "native" plant samples, allowing correct evaluation of our results, free of error and artifacts. Copyright © 2016 Elsevier Ltd. All rights reserved.

A correlative optical microscopy and scanning electron microscopy approach to locating nanoparticles in brain tumors.

PubMed

Kempen, Paul J; Kircher, Moritz F; de la Zerda, Adam; Zavaleta, Cristina L; Jokerst, Jesse V; Mellinghoff, Ingo K; Gambhir, Sanjiv S; Sinclair, Robert

2015-01-01

The growing use of nanoparticles in biomedical applications, including cancer diagnosis and treatment, demands the capability to exactly locate them within complex biological systems. In this work a correlative optical and scanning electron microscopy technique was developed to locate and observe multi-modal gold core nanoparticle accumulation in brain tumor models. Entire brain sections from mice containing orthotopic brain tumors injected intravenously with nanoparticles were imaged using both optical microscopy to identify the brain tumor, and scanning electron microscopy to identify the individual nanoparticles. Gold-based nanoparticles were readily identified in the scanning electron microscope using backscattered electron imaging as bright spots against a darker background. This information was then correlated to determine the exact location of the nanoparticles within the brain tissue. The nanoparticles were located only in areas that contained tumor cells, and not in the surrounding healthy brain tissue. This correlative technique provides a powerful method to relate the macro- and micro-scale features visible in light microscopy with the nanoscale features resolvable in scanning electron microscopy. Copyright © 2014 Elsevier Ltd. All rights reserved.

New developments in electron microscopy for serial image acquisition of neuronal profiles.

PubMed

Kubota, Yoshiyuki

2015-02-01

Recent developments in electron microscopy largely automate the continuous acquisition of serial electron micrographs (EMGs), previously achieved by laborious manual serial ultrathin sectioning using an ultramicrotome and ultrastructural image capture process with transmission electron microscopy. The new systems cut thin sections and capture serial EMGs automatically, allowing for acquisition of large data sets in a reasonably short time. The new methods are focused ion beam/scanning electron microscopy, ultramicrotome/serial block-face scanning electron microscopy, automated tape-collection ultramicrotome/scanning electron microscopy and transmission electron microscope camera array. In this review, their positive and negative aspects are discussed. © The Author 2015. Published by Oxford University Press on behalf of The Japanese Society of Microscopy. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

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.

Facilitating Research and Learning in Petrology and Geochemistry through Classroom Applications of Remotely Operable Research Instrumentation

NASA Astrophysics Data System (ADS)

Ryan, J. G.

2012-12-01

Bringing the use of cutting-edge research tools into student classroom experiences has long been a popular educational strategy in the geosciences and other STEM disciplines. The NSF CCLI and TUES programs have funded a large number of projects that placed research-grade instrumentation at educational institutions for instructional use and use in supporting undergraduate research activities. While student and faculty response to these activities has largely been positive, a range of challenges exist related to their educational effectiveness. Many of the obstacles these approaches have faced relate to "scaling up" of research mentoring experiences (e.g., providing training and time for use for an entire classroom of students, as opposed to one or two), and to time tradeoffs associated with providing technical training for effective instrument use versus course content coverage. The biggest challenge has often been simple logistics: a single instrument, housed in a different space, is difficult to integrate effectively into instructional activities. My CCLI-funded project sought primarily to knock down the logistical obstacles to research instrument use by taking advantage of remote instrument operation technologies, which allow the in-classroom use of networked analytical tools. Remote use of electron microprobe and SEM instruments of the Florida Center for Analytical Electron Microscopy (FCAEM) in Miami, FL was integrated into two geoscience courses at USF in Tampa, FL. Remote operation permitted the development of whole-class laboratory exercises to familiarize students with the tools, their function, and their capabilities; and it allowed students to collect high-quality chemical and image data on their own prepared samples in the classroom during laboratory periods. These activities improve student engagement in the course, appear to improve learning of key concepts in mineralogy and petrology, and have led to students pursuing independent research projects, as well as requesting additional Geology elective courses offering similar kinds of experiences. I have sustained these activities post-project via student lab fees to pay for in-class microprobe time.

Understanding Vesuvius magmatic processes: Evidence from primitive silicate-melt inclusions in medieval scoria clinopyroxenes (Terzigno formation)

USGS Publications Warehouse

Lima, A.; Belkin, H.E.; Torok, K.

1999-01-01

Microthermometric investigations of silicate-melt inclusions and electron microprobe analyses were conducted on experimentally homogenized silicate-melt inclusions and on the host clinopyroxenes from 4 scoria samples of different layers from the Mt. Somma-Vesuvius medieval eruption (Formazione di Terzigno, 893 A.D.). The temperature of homogenization, considered the minimum trapping temperature, ranges from 1190 to 1260??5 ??C for all clinopyroxene-hosted silicate melt inclusions. The major and minor-element compositional trends shown by Terzigno scoria and matrix glass chemical analysis are largely compatible with fractional crystallization of clinopyroxene and Fe-Ti oxides. Sulfur contents of the homogenized silicate-melt inclusions in clinopyroxene phenocrysts compared with that in the host scoria show that S has been significantly degassed in the erupted products; whereas, Cl has about the same abundance in the inclusions and in host scoria. Fluorine is low (infrequently up to 800 ppm) in the silicate-melt inclusions compared to 2400 ppm in the bulk scoria. Electron microprobe analyses of silicate-melt inclusions show that they have primitive magma compositions (Mg# = 75-91). The composition of the host clinopyroxene phenocrysts varies from typical plinian-related (Mg#???85) to non-plinian related (Mg#???85). The mixed source of the host clinopyroxenes and primitive nature of the silicate-melt inclusions implies that these phenocrysts, in part, may be residual and/or have a polygenetic origin. The similar variation trends of major and minor-elements between homogenized silicate-melt inclusions from the Terzigno scoria, and silicate-melt inclusions in olivine and diopside phenocrysts from plinian eruptions (Marianelli et al., 1995) suggest that the trapped inclusions represent melts similar to those that supplied the plinian and sub-plinian magma chambers. These geochemical characteristics suggest that the Vesuvius magmatic system retained a vestige of the most recent plinian event.

Onboard calibration igneous targets for the Mars Science Laboratory Curiosity rover and the Chemistry Camera laser induced breakdown spectroscopy instrument

NASA Astrophysics Data System (ADS)

Fabre, C.; Maurice, S.; Cousin, A.; Wiens, R. C.; Forni, O.; Sautter, V.; Guillaume, D.

2011-03-01

Accurate characterization of the Chemistry Camera (ChemCam) laser-induced breakdown spectroscopy (LIBS) on-board composition targets is of prime importance for the ChemCam instrument. The Mars Science Laboratory (MSL) science and operations teams expect ChemCam to provide the first compositional results at remote distances (1.5-7 m) during the in situ analyses of the Martian surface starting in 2012. Thus, establishing LIBS reference spectra from appropriate calibration standards must be undertaken diligently. Considering the global mineralogy of the Martian surface, and the possible landing sites, three specific compositions of igneous targets have been determined. Picritic, noritic, and shergottic glasses have been produced, along with a Macusanite natural glass. A sample of each target will fly on the MSL Curiosity rover deck, 1.56 m from the ChemCam instrument, and duplicates are available on the ground. Duplicates are considered to be identical, as the relative standard deviation (RSD) of the composition dispersion is around 8%. Electronic microprobe and laser ablation inductively coupled plasma mass spectrometry (LA ICP-MS) analyses give evidence that the chemical composition of the four silicate targets is very homogeneous at microscopic scales larger than the instrument spot size, with RSD < 5% for concentration variations > 0.1 wt.% using electronic microprobe, and < 10% for concentration variations > 0.01 wt.% using LA ICP-MS. The LIBS campaign on the igneous targets performed under flight-like Mars conditions establishes reference spectra for the entire mission. The LIBS spectra between 240 and 900 nm are extremely rich, hundreds of lines with high signal-to-noise, and a dynamical range sufficient to identify unambiguously major, minor and trace elements. For instance, a first LIBS calibration curve has been established for strontium from [Sr] = 284 ppm to [Sr] = 1480 ppm, showing the potential for the future calibrations for other major or minor elements.

Electron-microprobe study of chromitites associated with alpine ultramafic complexes and some genetic implications

USGS Publications Warehouse

Bird, M.L.

1978-01-01

Electron-microprobe and petrographic studies of alpine chromite deposits from around the world demonstrate that they are bimodal with respect to the chromic oxide content of their chromite. The two modes occur at 54 ? 4 and 37 ? 3 weight per cent chromic oxide corresponding to chromite designated as high-chromium and high-aluminum chromite respectively. The high-chromium chromite occurs exclusively with highly magnesian olivine (Fo92-97) and some interstitial diopside. The high-aluminum chromite is associated with more ferrous olivine (Fo88-92), diopside, enstatite, and feldspar. The plot of the mole ratios Cr/(Cr+Al+Fe3+) vs. Mg/(Mg+Fe2+) usually presented for alpine chromite is shown to have a high-chromium, high-iron to low-chromium, low-iron trend contrary to that shown by stratiform chromite. This trend is characteristic of alpine type chromite and is termed the alpine trend. However, a trend similar to that for startiform chromite is discernable on the graph for the high-chromium chromite data. This latter trend is well-developed at Red Mountain, Seldovia, Alaska. Analysis of the iron-magnesium distribution coefficient, Kd=(Fe/Mg)ol/(Fe/Mg)ch, between olivine and chromite shows that Kd for the high-chromium chromite from all ultramafic complexes has essentially the same constant value of .05 while the distribution coefficient for the high-aluminum chromite varies with composition of the chromite. These distribution coefficients are also characteristic of alpine-type chromites. The constant value for Kd for the high-chromium chromite and associated high-magnesium olivine in all alpine complexes suggests that they all crystallized under similar physico-chemical conditions. The two types of massive chromite and their associations of silicate minerals suggest the possibility of two populations with different origins. Recrystallization textures associated with the high-aluminum chromite together with field relationships between the gabbro and the chromite pods, suggest that the high-aluminum chromite was formed by metamorphic recrystallization of the ultramafic rocks and adjacent gabbro.

Precision controlled atomic resolution scanning transmission electron microscopy using spiral scan pathways

NASA Astrophysics Data System (ADS)

Sang, Xiahan; Lupini, Andrew R.; Ding, Jilai; Kalinin, Sergei V.; Jesse, Stephen; Unocic, Raymond R.

2017-03-01

Atomic-resolution imaging in an aberration-corrected scanning transmission electron microscope (STEM) can enable direct correlation between atomic structure and materials functionality. The fast and precise control of the STEM probe is, however, challenging because the true beam location deviates from the assigned location depending on the properties of the deflectors. To reduce these deviations, i.e. image distortions, we use spiral scanning paths, allowing precise control of a sub-Å sized electron probe within an aberration-corrected STEM. Although spiral scanning avoids the sudden changes in the beam location (fly-back distortion) present in conventional raster scans, it is not distortion-free. “Archimedean” spirals, with a constant angular frequency within each scan, are used to determine the characteristic response at different frequencies. We then show that such characteristic functions can be used to correct image distortions present in more complicated constant linear velocity spirals, where the frequency varies within each scan. Through the combined application of constant linear velocity scanning and beam path corrections, spiral scan images are shown to exhibit less scan distortion than conventional raster scan images. The methodology presented here will be useful for in situ STEM imaging at higher temporal resolution and for imaging beam sensitive materials.

Precision controlled atomic resolution scanning transmission electron microscopy using spiral scan pathways.

PubMed

Sang, Xiahan; Lupini, Andrew R; Ding, Jilai; Kalinin, Sergei V; Jesse, Stephen; Unocic, Raymond R

2017-03-08

Atomic-resolution imaging in an aberration-corrected scanning transmission electron microscope (STEM) can enable direct correlation between atomic structure and materials functionality. The fast and precise control of the STEM probe is, however, challenging because the true beam location deviates from the assigned location depending on the properties of the deflectors. To reduce these deviations, i.e. image distortions, we use spiral scanning paths, allowing precise control of a sub-Å sized electron probe within an aberration-corrected STEM. Although spiral scanning avoids the sudden changes in the beam location (fly-back distortion) present in conventional raster scans, it is not distortion-free. "Archimedean" spirals, with a constant angular frequency within each scan, are used to determine the characteristic response at different frequencies. We then show that such characteristic functions can be used to correct image distortions present in more complicated constant linear velocity spirals, where the frequency varies within each scan. Through the combined application of constant linear velocity scanning and beam path corrections, spiral scan images are shown to exhibit less scan distortion than conventional raster scan images. The methodology presented here will be useful for in situ STEM imaging at higher temporal resolution and for imaging beam sensitive materials.

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.

Development of near-field scanning microwave and optical dual probe: Application to characterization of high-T(c) superconductors

NASA Astrophysics Data System (ADS)

Aga, Roberto Sabas, Jr.

In this dissertation, a novel dual-channel near-field scanning microwave and optical microprobe (NSMM/NSOM) was developed for simultaneous mapping of microwave and optical properties of a sample at microscopic scales. This microprobe is composed of an open-end coaxial resonator with its center conductor being replaced by a stainless steel tube terminated by a titanium/silver coated fiber optic with a tapered tip. The optical fiber serves as the channel for NSOM, while its metal coating is the channel for NSMM. Using this dual-channel NSMM/NSOM probe, a spatial resolution of ˜5 mum, that is comparable to the best reported for single-channel NSMM, has been achieved on metallic samples. This resolution is mainly limited by the sensitivity of the NSMM channel and may be further improved when the sensitivity of NSMM is enhanced. Characterization of the microwave properties of the highest-Tc Hg-based superconductors has been carried out using a traditional resonant cavity technique, as well as a novel single-channel NSMM and the dual-channel NSMM/NSOM. Using the traditional technique, the microwave surface resistance (Rs) and power handling capability (Pc) of HgBa 2CaCu2O6 (Hg-1212 with Tc ˜ 125 K) films have been measured for the first time, and the results are superior to the best achieved on other superconductors. For example, a comparable R s ˜ 0.3 mO (10 GHz) can be obtained on Hg-1212 at close to 120 K as opposed to the same Rs for YBa2Cu3O 7 (the most popular high-Tc superconductor with Tc ˜ 92 K) at around 77K. This can be attributed to the large difference in the Tcs between the two materials and has demonstrated the potential of Hg-1212 for microwave applications. A comparison of the microwave properties of Hg-1212, Tl-2212 and YBCO films at reduced temperature scale suggested further room for improvement of Hg-1212 performance. Using NSMM, the localized microwave properties, such as Tcs, sheet resistance and power handling capability have been investigated and nonuniformity, revealed. Attempts to correlate the observed nonuniformity of microwave properties with the microstructures of the sample have been made using the dual-channel NSMM/NSOM probe and interesting results, obtained. (Abstract shortened by UMI.)

The Scanning Electron Microscope and the Archaeologist

ERIC Educational Resources Information Center

Ponting, Matthew

2004-01-01

Images from scanning electron microscopy are now quite common and they can be of great value in archaeology. Techniques such as secondary electron imaging, backscattered electron imaging and energy-dispersive x-ray analysis can reveal information such as the presence of weevils in grain in Roman Britain, the composition of Roman coins and the…

Laser ablation ICP-MS analysis on nano-powder pellets and applications to granite bulk rock analysis

NASA Astrophysics Data System (ADS)

Wu, Shitou; Karius, Volker; Wörner, Gerhard

2017-04-01

Granites are a ubiquitous component of the continental crust and knowing their precise trace element signatures is essential in understanding the origins and evolution of the continental crust. ICP-MS bulk analysis of granite is generally conducted on solution after acid-digestion. However this technique has several deficiencies related to the difficulty of completely dissolving accessary minerals such as zircon and the instability/adsorption of high valence trace elements (Nb, Ta et al.) in acid solutions. The development of a nano-powder pellet technique by using wet milling procedure, and its combination with laser ablation ICP-MS has been proposed to overcome these problems. In this study, we produced nano-powders from a series of granite rock standards by wet milling in agate using a high power planetary ball mill instrument. The procedure was tested and optimized by modifying parameters (ball to powder ratio, water to powder ratio, milling power etc.). Characterization of nano-powders was conducted by various techniques including electron microprobe (EMP), secondary electron imaging, polarizing microscope, and laser particle size analyzer (LPSA) and laser scanning confocal microscope (LSCM). Particle sizes range from a few nm to 5 μm with a small secondary mode at around 10 to 20 μm that probably represent particle aggregates rather than remaining crystal grains after milling. Pellets of 5 mm in diameter were pressed into molds of cellulose at 1.75 *103 N/cm2. Surface roughness of the pellets was measured by LSCM and gave a Ra of 0.494 μm, which is an order higher than the surface of polished ATGH-G reference glass surface (Ra: 0.048 μm), but sufficient for laser ablation. Sources of contamination either from abrading agate balls or from ultrapure water were evaluated and quantified. The homogeneity of powder pellets down to less than 5 μm size was documented based on EMPA element mapping and statistical analyses of LA-ICP-MS in discrete spot and line scanning analytical mode. We report data from major to trace element (to < 0.1 ppm) of currently available international granite reference materials (JG-2, JG-3, GWB07103, GEB07111, GSP-2 and G-3) to evaluate analytical precision and accuracy of LA-ICP-MS measurements. Our results illustrate the potential of this method for high precision analysis of trace elements and e.g. Zr/Hf and Nb/Ta ratios in granites.

Scanning Electron Microscopy (SEM) Procedure for HE Powders on a Zeiss Sigma HD VP SEM

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

Zaka, F.

This method describes the characterization of inert and HE materials by the Zeiss Sigma HD VP field emission Scanning Electron Microscope (SEM). The SEM uses an accelerated electron beam to generate high-magnification images of explosives and other materials. It is fitted with five detectors (SE, Inlens, STEM, VPSE, HDBSD) to enable imaging of the sample via different secondary electron signatures, angles, and energies. In addition to imaging through electron detection, the microscope is also fitted with two Oxford Instrument Energy Dispersive Spectrometer (EDS) 80 mm detectors to generate elemental constituent spectra and two-dimensional maps of the material being scanned.

Comparative study of image contrast in scanning electron microscope and helium ion microscope.

PubMed

O'Connell, R; Chen, Y; Zhang, H; Zhou, Y; Fox, D; Maguire, P; Wang, J J; Rodenburg, C

2017-12-01

Images of Ga + -implanted amorphous silicon layers in a 110 n-type silicon substrate have been collected by a range of detectors in a scanning electron microscope and a helium ion microscope. The effects of the implantation dose and imaging parameters (beam energy, dwell time, etc.) on the image contrast were investigated. We demonstrate a similar relationship for both the helium ion microscope Everhart-Thornley and scanning electron microscope Inlens detectors between the contrast of the images and the Ga + density and imaging parameters. These results also show that dynamic charging effects have a significant impact on the quantification of the helium ion microscope and scanning electron microscope contrast. © 2017 The Authors Journal of Microscopy © 2017 Royal Microscopical Society.

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

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.

New concept of a submillimetric pixellated Silicon detector for intracerebral application

NASA Astrophysics Data System (ADS)

Benoit, M.; Märk, J.; Weiss, P.; Benoit, D.; Clemens, J. C.; Fougeron, D.; Janvier, B.; Jevaud, M.; Karkar, S.; Menouni, M.; Pain, F.; Pinot, L.; Morel, C.; Laniece, P.

2011-12-01

A new beta+ radiosensitive microprobe implantable in rodent brain dedicated to in vivo and autonomous measurements of local time activity curves of beta radiotracers in a volume of brain tissue of a few mm3 has been developed recently. This project expands the concept of the previously designed beta microprobe, which has been validated extensively in neurobiological experiments performed on anesthetized animals. Due to its limitations considering recordings on awake and freely moving animals, we have proposed to develop a wireless setup that can be worn by an animal without constraining its movements. To that aim, we have chosen a highly beta sensitive Silicon-based detector to devise a compact pixellated probe. Miniaturized wireless electronics is used to read-out and transfer the measurement data. Initial Monte-Carlo simulations showed that high resistive Silicon pixels are appropriate for this purpose, with their dimensions to be adapted to our specific signals. More precisely, we demonstrated that 200 μm thick pixels with an area of 200 μm×500 μm are optimized in terms of beta+sensitivity versus relative transparency to the gamma background. Based on this theoretical study, we now present the development of the novel sensor, including the system simulations with technology computer-assisted design (TCAD) to investigate specific configurations of guard rings and their potential to increase the electrical isolation and stabilization of the pixel, as well as the corresponding physical tests to validate the particular geometries of this new sensor.

Iron and nickel isotope fractionation by diffusion, with applications to iron meteorites

NASA Astrophysics Data System (ADS)

Watson, Heather C.; Richter, Frank; Liu, Ankun; Huss, Gary R.

2016-10-01

Mass-dependent, kinetic fractionation of isotopes through processes such as diffusion can result in measurable isotopic signatures. When these signatures are retained in geologic materials, they can be used to help interpret their thermal histories. The mass dependence of the diffusion coefficient of isotopes 1 and 2 can be written as (D1 /D2) =(m2 /m1) β, where D1 and D2 are the diffusion coefficients of m1 and m2 respectively, and β is an empirical coefficient that relates the two ratios. Experiments have been performed to measure β in the Fe-Ni alloy system. Diffusion couple experiments between pure Fe and Ni metals were run in a piston cylinder at 1300-1400 °C and 1 GPa. Concentration and isotopic profiles were measured by electron microprobe and ion microprobe respectively. We find that a single β coefficient of β = 0.32 ± 0.04 can describe the isotopic effect in all experiments. This result is comparable to the isotope effect determined in many other similar alloy systems. The new β coefficient is used in a model of the isotopic profiles to be expected during the Widmanstätten pattern formation in iron meteorites. The results are consistent with previous estimates of the cooling rate of the iron meteorite Toluca. The application of isotopic constraints based on these results in addition to conventional cooling rate models could provide a more robust picture of the thermal history of these early planetary bodies.

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.

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.

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.

Petrography of the carbonaceous, diamond-bearing stone "Hypatia" from southwest Egypt: A contribution to the debate on its origin

NASA Astrophysics Data System (ADS)

Belyanin, Georgy A.; Kramers, Jan D.; Andreoli, Marco A. G.; Greco, Francesco; Gucsik, Arnold; Makhubela, Tebogo V.; Przybylowicz, Wojciech J.; Wiedenbeck, Michael

2018-02-01

The stone named "Hypatia" found in the Libyan Desert Glass area of southwest Egypt is carbon-dominated and rich in microdiamonds. Previous noble gas and nitrogen isotope studies suggest an extraterrestrial origin. We report on a reconnaissance study of the carbonaceous matrix of this stone and the phases enclosed in it. This focused on areas not affected by numerous transecting fractures mostly filled with secondary minerals. The work employed scanning electron microscopy (SEM) with energy-dispersive (EDS) and wavelength-dispersive (WDS) electron microprobe (EMPA) analysis, Proton Induced X-ray Emission (PIXE) spectrometry and micro-Raman spectroscopy. We found that carbonaceous matrices of two types occur irregularly intermingled on the 50-500 μm scale: Matrix-1, consisting of almost pure carbonaceous matter, and Matrix-2, containing Fe, Ni, P and S at abundances analyzable by microprobe. Matrix-2 contains the following phases as inclusions: (i) (Fe,Ni) sulphide occurring in cloud-like concentrations of sub-μm grains, in domains of the matrix that are enriched in Fe and S. These domains have (Fe + Ni)/S (atomic) = 1.51 ± 0.24 and Ni/Fe = 0.086 ± 0.061 (both 1SD); (ii) grains up to ∼5 μm in size of moissanite (SiC); (iii) Ni-phosphide compound grains up to 60 μm across that appear cryptocrystalline or amorphous and have (Ni + Fe)/P (atomic) = 5.6. ± 1.7 and Ni/Fe = 74 ± 29 (both 1SD), where both these ratios are much higher than any known Ni-phosphide minerals; (iv) rare grains (observed only once) of graphite, metallic Al, Fe and Ag, and a phase consisting of Ag, P and I. In Matrix-2, Raman spectroscopy shows a prominent narrow diamond band at 1340 cm-1. In Matrix-1 the D and G bands of disordered carbon are dominant, but a minor diamond band is ubiquitous, accounting for the uniform hardness of the material. The D and G bands have average full width at half maximum (FWHM) values of 295 ± 19 and 115 ± 19 cm-1, respectively, and the D/G intensity ratio is 0.75 ± 0.09 (both 1SD). These values are similar to those of the most primitive solar system carbonaceous matter. The diamond phase is considered to be a product of shock. The (Fe, Ni) sulphide phase is probably pyrrhotite and a shock origin is likewise proposed for it. Moissanite is frequently associated with the Ni-phosphide phase, and a presolar origin for both is suggested. The lack of recrystallization of the Ni-phosphide phase suggests that the Hypatia stone did not experience long-lasting thermal metamorphism, in accord with the Raman D-G band characteristics. A lack of silicate matter sets the stone apart from interplanetary dust particles and known cometary material. This, along with the dual intermingled matrices internal to it, could indicate a high degree of heterogeneity in the early solar nebula.

U-Pb geochronology of zircon and polygenetic titanite from the Glastonbury Complex, Connecticut, USA: An integrated SEM, EMPA, TIMS, and SHRIMP study

USGS Publications Warehouse

Aleinikoff, J.N.; Wintsch, R.P.; Fanning, C.M.; Dorais, M.J.

2002-01-01

U-Pb ages for zircon and titanite from a granodioritic gneiss in the Glastonbury Complex, Connecticut, have been determined using both isotope dilution thermal ionization mass spectrometry (TIMS) and the sensitive high resolution ion microprobe (SHRIMP). Zircons occur in three morphologic populations: (1) equant to stubby, multifaceted, colorless, (2) prismatic, dark brown, with numerous cracks, and (3) elongate, prismatic, light tan to colorless. Cathodoluminescence (CL) imaging of the three populations shows simple concentric oscillatory zoning. The zircon TIMS age [weighted average of 207Pb/206Pb ages from Group 3 grains-450.5 ?? 1.6 Ma (MSWD=1.11)] and SHRIMP age [composite of 206Pb/238 U age data from all three groups-448.2 ?? 2.7 Ma (MSWD = 1.3)], are interpreted to suggest a relatively simple crystallization history. Titanite from the granodioritic gneiss occurs as both brown and colorless varieties. Scanning electron microscope backscatter (BSE) images of brown grains show multiple cross-cutting oscillatory zones of variable brightness and dark overgrowths. Colorless grains are unzoned or contain subtle wispy or very faint oscillatory zoning. Electron microprobe analysis (EMPA) clearly distinguishes the two populations. Brown grains contain relatively high concentrations of Fe2O3, Ce2O3 (up to ~ 1.5 wt.%), Nb2O5, and Zr. Cerium concentration is positively correlated with total REE + Y concentration, which together can exceed 3.5 wt.%. Oscillatory zoning in brown titanite is correlated with variations in REE concentrations. In contrast, colorless titanite (both as discrete grains and overgrowths on brown titanite) contains lower concentrations of Y, REE, Fe2O3, and Zr, but somewhat higher Al2O3 and Nb2O5. Uranium concentrations and Th/U discriminate between brown grains (typically 200-400 ppm U; all analyses but one have Th/U between about 0.8 and 2) and colorless grains (10-60 ppm U; Th/U of 0-0.17). In contrast to the zircon U-Pb age results, SHRIMP U-Pb data from titanite indicate multiple growth episodes. In brown grains, oscillatory zoned cores formed at 443 ?? 6 Ma, whereas white (in BSE) cross-cutting zones are 425 ?? 9 Ma. Colorless grains and overgrowths on brown grains yield an age of 265 ?? 8 Ma (using the Total Pb method) or 265 ?? 5 Ma (using the weighted average of the 206Pb/238U ages). However, EMPA chemical data identify zoning that suggests that this colorless titanite may preserve three growth events. Oscillatory zoned portions of brown titanite grains are igneous in origin; white cross-cutting zones probably formed during a previously unrecognized event that caused partial dissolution of earlier titanite and reprecipitation of a slightly younger generation of brown titanite. Colorless titanite replaced and grew over the magmatic titanite during the Permian Alleghanian orogeny. These isotopic data indicate that titanite, like zircon, can contain multiple age components. Coupling SHRIMP microanalysis with EMPA and SEM results on dated zones as presented in this study is an efficient and effective technique to extract additional chronologic ?? 2002 Elsevier Science B.V. All rights reserved.

Correction of image drift and distortion in a scanning electron microscopy.

PubMed

Jin, P; Li, X

2015-12-01

Continuous research on small-scale mechanical structures and systems has attracted strong demand for ultrafine deformation and strain measurements. Conventional optical microscope cannot meet such requirements owing to its lower spatial resolution. Therefore, high-resolution scanning electron microscope has become the preferred system for high spatial resolution imaging and measurements. However, scanning electron microscope usually is contaminated by distortion and drift aberrations which cause serious errors to precise imaging and measurements of tiny structures. This paper develops a new method to correct drift and distortion aberrations of scanning electron microscope images, and evaluates the effect of correction by comparing corrected images with scanning electron microscope image of a standard sample. The drift correction is based on the interpolation scheme, where a series of images are captured at one location of the sample and perform image correlation between the first image and the consequent images to interpolate the drift-time relationship of scanning electron microscope images. The distortion correction employs the axial symmetry model of charged particle imaging theory to two images sharing with the same location of one object under different imaging fields of view. The difference apart from rigid displacement between the mentioned two images will give distortion parameters. Three-order precision is considered in the model and experiment shows that one pixel maximum correction is obtained for the employed high-resolution electron microscopic system. © 2015 The Authors Journal of Microscopy © 2015 Royal Microscopical Society.

High-resolution, high-throughput imaging with a multibeam scanning electron microscope.

PubMed

Eberle, A L; Mikula, S; Schalek, R; Lichtman, J; Knothe Tate, M L; Zeidler, D

2015-08-01

Electron-electron interactions and detector bandwidth limit the maximal imaging speed of single-beam scanning electron microscopes. We use multiple electron beams in a single column and detect secondary electrons in parallel to increase the imaging speed by close to two orders of magnitude and demonstrate imaging for a variety of samples ranging from biological brain tissue to semiconductor wafers. © 2015 The Authors Journal of Microscopy © 2015 Royal Microscopical Society.

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.

Dynamic scan control in STEM: Spiral scans

DOE PAGES

Lupini, Andrew R.; Borisevich, Albina Y.; Kalinin, Sergei V.; ...

2016-06-13

Here, scanning transmission electron microscopy (STEM) has emerged as one of the foremost techniques to analyze materials at atomic resolution. However, two practical difficulties inherent to STEM imaging are: radiation damage imparted by the electron beam, which can potentially damage or otherwise modify the specimen and slow-scan image acquisition, which limits the ability to capture dynamic changes at high temporal resolution. Furthermore, due in part to scan flyback corrections, typical raster scan methods result in an uneven distribution of dose across the scanned area. A method to allow extremely fast scanning with a uniform residence time would enable imaging atmore » low electron doses, ameliorating radiation damage and at the same time permitting image acquisition at higher frame-rates while maintaining atomic resolution. The practical complication is that rastering the STEM probe at higher speeds causes significant image distortions. Non-square scan patterns provide a solution to this dilemma and can be tailored for low dose imaging conditions. Here, we develop a method for imaging with alternative scan patterns and investigate their performance at very high scan speeds. A general analysis for spiral scanning is presented here for the following spiral scan functions: Archimedean, Fermat, and constant linear velocity spirals, which were tested for STEM imaging. The quality of spiral scan STEM images is generally comparable with STEM images from conventional raster scans, and the dose uniformity can be improved.« less

Dynamic scan control in STEM: Spiral scans

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

Lupini, Andrew R.; Borisevich, Albina Y.; Kalinin, Sergei V.

Here, scanning transmission electron microscopy (STEM) has emerged as one of the foremost techniques to analyze materials at atomic resolution. However, two practical difficulties inherent to STEM imaging are: radiation damage imparted by the electron beam, which can potentially damage or otherwise modify the specimen and slow-scan image acquisition, which limits the ability to capture dynamic changes at high temporal resolution. Furthermore, due in part to scan flyback corrections, typical raster scan methods result in an uneven distribution of dose across the scanned area. A method to allow extremely fast scanning with a uniform residence time would enable imaging atmore » low electron doses, ameliorating radiation damage and at the same time permitting image acquisition at higher frame-rates while maintaining atomic resolution. The practical complication is that rastering the STEM probe at higher speeds causes significant image distortions. Non-square scan patterns provide a solution to this dilemma and can be tailored for low dose imaging conditions. Here, we develop a method for imaging with alternative scan patterns and investigate their performance at very high scan speeds. A general analysis for spiral scanning is presented here for the following spiral scan functions: Archimedean, Fermat, and constant linear velocity spirals, which were tested for STEM imaging. The quality of spiral scan STEM images is generally comparable with STEM images from conventional raster scans, and the dose uniformity can be improved.« less

Expansion of Shockley stacking fault observed by scanning electron microscope and partial dislocation motion in 4H-SiC

NASA Astrophysics Data System (ADS)

Yamashita, Yoshifumi; Nakata, Ryu; Nishikawa, Takeshi; Hada, Masaki; Hayashi, Yasuhiko

2018-04-01

We studied the dynamics of the expansion of a Shockley-type stacking fault (SSF) with 30° Si(g) partial dislocations (PDs) using a scanning electron microscope. We observed SSFs as dark lines (DLs), which formed the contrast at the intersection between the surface and the SSF on the (0001) face inclined by 8° from the surface. We performed experiments at different electron-beam scanning speeds, observing magnifications, and irradiation areas. The results indicated that the elongation of a DL during one-frame scanning depended on the time for which the electron beam irradiated the PD segment in the frame of view. From these results, we derived a formula to express the velocity of the PD using the elongation rate of the corresponding DL during one-frame scanning. We also obtained the result that the elongation velocity of the DL was not influenced by changing the direction in which the electron beam irradiates the PD. From this result, we deduced that the geometrical kink motion of the PD was enhanced by diffusing carriers that were generated by the electron-beam irradiation.

Three-dimensional imaging of adherent cells using FIB/SEM and STEM.

PubMed

Villinger, Clarissa; Schauflinger, Martin; Gregorius, Heiko; Kranz, Christine; Höhn, Katharina; Nafeey, Soufi; Walther, Paul

2014-01-01

In this chapter we describe three different approaches for three-dimensional imaging of electron microscopic samples: serial sectioning transmission electron microscopy (TEM), scanning transmission electron microscopy (STEM) tomography, and focused ion beam/scanning electron microscopy (FIB/SEM) tomography. With these methods, relatively large volumes of resin-embedded biological structures can be analyzed at resolutions of a few nm within a reasonable expenditure of time. The traditional method is serial sectioning and imaging the same area in all sections. Another method is TEM tomography that involves tilting a section in the electron beam and then reconstruction of the volume by back projection of the images. When the scanning transmission (STEM) mode is used, thicker sections (up to 1 μm) can be analyzed. The third approach presented here is focused ion beam/scanning electron microscopy (FIB/SEM) tomography, in which a sample is repeatedly milled with a focused ion beam (FIB) and each newly produced block face is imaged with the scanning electron microscope (SEM). This process can be repeated ad libitum in arbitrary small increments allowing 3D analysis of relatively large volumes such as eukaryotic cells. We show that resolution of this approach is considerably improved when the secondary electron signal is used. However, the most important prerequisite for three-dimensional imaging is good specimen preparation. For all three imaging methods, cryo-fixed (high-pressure frozen) and freeze-substituted samples have been used.

Mineralized soft-tissue structure and chemistry in a mummified hadrosaur from the Hell Creek Formation, North Dakota (USA).

PubMed

Manning, Phillip L; Morris, Peter M; McMahon, Adam; Jones, Emrys; Gize, Andy; Macquaker, Joe H S; Wolff, George; Thompson, Anu; Marshall, Jim; Taylor, Kevin G; Lyson, Tyler; Gaskell, Simon; Reamtong, Onrapak; Sellers, William I; van Dongen, Bart E; Buckley, Mike; Wogelius, Roy A

2009-10-07

An extremely well-preserved dinosaur (Cf. Edmontosaurus sp.) found in the Hell Creek Formation (Upper Cretaceous, North Dakota) retains soft-tissue replacement structures and associated organic compounds. Mineral cements precipitated in the skin apparently follow original cell boundaries, partially preserving epidermis microstructure. Infrared and electron microprobe images of ossified tendon clearly show preserved mineral zonation, with silica and trapped carbon dioxide forming thin linings on Haversian canals within apatite. Furthermore, Fourier transform infrared spectroscopy (FTIR) of materials recovered from the skin and terminal ungual phalanx suggests the presence of compounds containing amide groups. Amino acid composition analyses of the mineralized skin envelope clearly differ from the surrounding matrix; however, intact proteins could not be obtained using protein mass spectrometry. The presence of endogenously derived organics from the skin was further demonstrated by pyrolysis gas chromatography mass spectrometry (Py-GCMS), indicating survival and presence of macromolecules that were in part aliphatic (see the electronic supplementary material).

Mineralized soft-tissue structure and chemistry in a mummified hadrosaur from the Hell Creek Formation, North Dakota (USA)

PubMed Central

Manning, Phillip L.; Morris, Peter M.; McMahon, Adam; Jones, Emrys; Gize, Andy; Macquaker, Joe H. S.; Wolff, George; Thompson, Anu; Marshall, Jim; Taylor, Kevin G.; Lyson, Tyler; Gaskell, Simon; Reamtong, Onrapak; Sellers, William I.; van Dongen, Bart E.; Buckley, Mike; Wogelius, Roy A.

2009-01-01

An extremely well-preserved dinosaur (Cf. Edmontosaurus sp.) found in the Hell Creek Formation (Upper Cretaceous, North Dakota) retains soft-tissue replacement structures and associated organic compounds. Mineral cements precipitated in the skin apparently follow original cell boundaries, partially preserving epidermis microstructure. Infrared and electron microprobe images of ossified tendon clearly show preserved mineral zonation, with silica and trapped carbon dioxide forming thin linings on Haversian canals within apatite. Furthermore, Fourier transform infrared spectroscopy (FTIR) of materials recovered from the skin and terminal ungual phalanx suggests the presence of compounds containing amide groups. Amino acid composition analyses of the mineralized skin envelope clearly differ from the surrounding matrix; however, intact proteins could not be obtained using protein mass spectrometry. The presence of endogenously derived organics from the skin was further demonstrated by pyrolysis gas chromatography mass spectrometry (Py-GCMS), indicating survival and presence of macromolecules that were in part aliphatic (see the electronic supplementary material). PMID:19570788

Single agglutinates: A comparative study of compositions of agglutinitic glass, whole-grain, bulk soil, and FMR

NASA Technical Reports Server (NTRS)

Basu, A.; Robinson, R.; Mckay, D. S.; Blanchard, D. P.; Morris, R. V.; Wentworth, Susan J.

1994-01-01

Previous workers on single agglutinates have variously interpreted the composition of agglutinitic glass to represent impact melts of (1) bulk soil, (2) mixed components in finer sizes, and (3) microtargets. Separately, Papike has argued in favor of fusion of the finest fraction of bulk soils. Thirty-four single agglutinates were hand-picked from the mature Apollo 16 soil 61181 (I(sub s)/FeO = 82) and the FMR and chemical composition (INAA for Fe, Sc, Sm, Co, Ni, and Cr) of each agglutinate particle were measured. Thirteen of these single agglutinates were selected for electron beam microanalysis and imaging. Less than 1 micron spots were analyzed (for Na, Mg, Al, Si, P, S, K, Ca, Ti, Cr, Mn, Fe, Ni, and Ba) on pure glassy areas (approximately ten in each particle) selected on the basis of optical and BSE images (avoiding all clasts and inclusions) with an electron microprobe to obtain average glass compositions of each single agglutinate.

Lunar highland rocks - Element partitioning among minerals. II - Electron microprobe analyses of Al, P, Ca, Ti, Cr, Mn and Fe in olivine

NASA Technical Reports Server (NTRS)

Smith, J. V.; Hansen, E. C.; Steele, I. M.

1980-01-01

Lunar olivines from anorthosites, granulitic impactites, and rocks in the Mg-rich plutonic trend were subjected to electron probe measurements for Al, P, Ca, Ti, Cr and Mn, which show that the FeO/MnO ratio for lunar olivines lies between 80 and 110 with little difference among the rock types. The low values of Ca in lunar olivines indicate slow cooling to subsolidus temperatures, with blocking temperatures of about 750 C for 67667 and 1000 C for 60255,73-alpha determined by the Finnerty and Boyd (1978) experiments. An important paradox is noted in the low Ti content of Fe-rich olivines from anorthosites, although both Ti and Fe tend to become enriched in liquid during fractional distillation. Except for Ca and Mn, olivine from anorthosites has lower minor element values than other rock types. Formation from a chemically distinct system is therefore implied.