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  • 1
    Electronic Resource
    Electronic Resource
    [S.l.] : American Institute of Physics (AIP)
    Review of Scientific Instruments 60 (1989), S. 1686-1689 
    ISSN: 1089-7623
    Source: AIP Digital Archive
    Topics: Physics , Electrical Engineering, Measurement and Control Technology
    Notes: The capabilities of a direct imaging photoelectron microscope (MicroESCA from Surface Science Instruments) have been demonstrated in a set of experiments carried out at the Stanford Synchrotron Radiation Laboratory (SSRL) using a torroidal grating monochromator in the photon energy range 20–170 eV. Photoelectrons from a 300×300 μm2 sample area are projected in the diverging magnetic field of a superconducting solenoid and an image reflecting the variation in photoelectron yield is recorded digitally with a resistive anode imaging detector. Lateral resolution is better than 5 μm. A retarding field analyzer located in front of the imaging detector acts as a high-pass filter and allows us to obtain a series of spectrally resolved images which can be processed to give a spot XPS analysis of areas as small as 5×5 μm2. Images from a sample of patterned aluminum on silicon are presented to demonstrate the potential of the instrument.
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  • 2
    Electronic Resource
    Electronic Resource
    Springer
    Contributions to mineralogy and petrology 125 (1996), S. 311-318 
    ISSN: 1432-0967
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences
    Notes: Abstract  Infrared spectroscopy provides a reliable method for rapid, non-destructive quantitative analysis of volatile species in silicate glasses, with applications to geochemistry and volcanology. The technique has been extensively calibrated for transmission measurements, in which the species concentration present is correlated with the height or area of characteristic absorption peaks, for doubly polished samples of known thickness. There are several drawbacks associated with this method, including the need for double polishing of parallel faces on thin samples, the errors associated with sample thickness measurement, and total absorption of the IR beam intensity for samples with high volatile content. We have tested an alternative method for quantitative IR determination of volatile concentrations in silicate glasses, based on analysis of the IR reflectivity signal. The reflectivity method requires preparation of a single polished glass surface, and no thickness measurement of the sample is necessary. The technique is applied easily as a microbeam technique using apertures as small as a few μm in diameter. The method should be particularly useful for volatile analysis of glass inclusions in phenocrystals, or standard samples in thin section. We have developed the methodology for the technique using a series of basanite and leucitite glasses with high carbonate contents (〉1 wt% CO2), which could not be easily analyzed via IR transmission. We have used SIMS to standardize the technique. Two features observed in the reflectance spectra near 1400 cm–1 and 1500 cm–1 are due to resonance of the infrared beam with the asymmetric stretching vibrations of carbonate groups. The contribution of these species to the total reflectivity is directly correlated with the carbon abundance in the samples. This forms the basis for an empirical quantitative analysis. The optical constants, including the IR absorption coefficients associated with the CO3 2– stretching vibrations, have been extracted by Kramers-Kronig analysis of the reflectivity data. The molar extinction coefficients are 1119 ± 138 L mol–1 cm–1 and 1198 ± 145 L mol–1 cm–1 for the 1400 and 1500 cm–1 bands, respectively, in excellent agreement with results of previous transmission studies, after orientation effects are taken into account.
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  • 3
    Electronic Resource
    Electronic Resource
    Springer
    Journal of applied electrochemistry 2 (1972), S. 23-29 
    ISSN: 1572-8838
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology , Electrical Engineering, Measurement and Control Technology
    Notes: Abstract The simple optical cell described is useful for providing supplementary information on the evolution of gases during the electrolysis of fused salts or other electrolytes. Its use with PbS-PbCl2 and PbS-PbCl2-NaCl melts demonstrated that, for anodic sulphur gas production, residual gas evolution occurs, indicating the formation of a chemisorbed species as a reaction intermediate. Dissolution of the sulphur in the melt also takes place; its rate increases with increase in temperature and sulphide concentration.
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  • 4
    Publication Date: 1989-07-01
    Print ISSN: 0034-6748
    Electronic ISSN: 1089-7623
    Topics: Electrical Engineering, Measurement and Control Technology , Physics
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  • 5
    Publication Date: 2015-04-02
    Description: The Mars Science Laboratory (MSL) rover Curiosity has documented a section of fluvio-lacustrine strata at Yellowknife Bay (YKB), an embayment on the floor of Gale crater, approximately 500 m east of the Bradbury landing site. X-ray diffraction (XRD) data and evolved gas analysis (EGA) data from the CheMin and SAM instruments show that two powdered mudstone samples (named John Klein and Cumberland) drilled from the Sheepbed member of this succession contain up to ~20 wt% clay minerals. A trioctahedral smectite, likely a ferrian saponite, is the only clay mineral phase detected in these samples. Smectites of the two samples exhibit different 001 spacing under the low partial pressures of H 2 O inside the CheMin instrument (relative humidity 〈1%). Smectite interlayers in John Klein collapsed sometime between clay mineral formation and the time of analysis to a basal spacing of 10 Å, but largely remain open in the Cumberland sample with a basal spacing of ~13.2 Å. Partial intercalation of Cumberland smectites by metal-hydroxyl groups, a common process in certain pedogenic and lacustrine settings on Earth, is our favored explanation for these differences. The relatively low abundances of olivine and enriched levels of magnetite in the Sheepbed mudstone, when compared with regional basalt compositions derived from orbital data, suggest that clay minerals formed with magnetite in situ via aqueous alteration of olivine. Mass-balance calculations are permissive of such a reaction. Moreover, the Sheepbed mudstone mineral assemblage is consistent with minimal inputs of detrital clay minerals from the crater walls and rim. Early diagenetic fabrics suggest clay mineral formation prior to lithification. Thermodynamic modeling indicates that the production of authigenic magnetite and saponite at surficial temperatures requires a moderate supply of oxidants, allowing circum-neutral pH. The kinetics of olivine alteration suggest the presence of fluids for thousands to hundreds of thousands of years. Mineralogical evidence of the persistence of benign aqueous conditions at YKB for extended periods indicates a potentially habitable environment where life could establish itself. Mediated oxidation of Fe 2+ in olivine to Fe 3+ in magnetite, and perhaps in smectites provided a potential energy source for organisms.
    Print ISSN: 0003-004X
    Electronic ISSN: 1945-3027
    Topics: Geosciences
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  • 6
    Publication Date: 2014-12-24
    Description: Sulfate minerals are important indicators for aqueous geochemical environments. The geology and mineralogy of Mars have been studied through the use of various remote-sensing techniques, including thermal (mid-infrared) emission and visible/near-infrared reflectance spectroscopies. Spectral analyses of spacecraft data (from orbital and landed missions) using these techniques have indicated the presence of sulfate minerals on Mars, including Fe-rich sulfates on the iron-rich planet. Each individual Fe-sulfate mineral can be used to constrain bulk chemistry and lends more information about the specific formational environment [e.g., Fe 2+ sulfates are typically more water soluble than Fe 3+ sulfates and their presence would imply a water-limited (and lower Eh) environment; Fe 3+ sulfates form over a range of hydration levels and indicate further oxidation (biological or abiological) and increased acidification]. To enable better interpretation of past and future terrestrial or planetary data sets, with respect to the Fe-sulfates, we present a comprehensive collection of mid-infrared thermal emission (2000 to 220 cm –1 ; 5–45 μm) and visible/near-infrared (0.35–5 μm) spectra of 21 different ferrous- and ferric-iron sulfate minerals. Mid-infrared vibrational modes (for SO 4 , OH, H 2 O) are assigned to each thermal emissivity spectrum, and the electronic excitation and transfer bands and vibrational OH, H 2 O, and SO 4 overtone and combination bands are assigned to the visible/near-infrared reflectance spectra. Presentation and characterization of these Fe-sulfate thermal emission and visible/near-infrared reflectance spectra will enable the specific chemical environments to be determined when individual Fe-sulfate minerals are identified.
    Print ISSN: 0003-004X
    Electronic ISSN: 1945-3027
    Topics: Geosciences
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  • 7
    Publication Date: 2014-06-27
    Description: Microbialites form the earliest macroscopic evidence of life, and have always been important in particular aquatic ecosystems. They demonstrate the remarkable ability of microorganisms to provide the foundation for structures that can rival coral reefs in size. Microbialites are generally assumed to form by microbial trapping and binding of detrital grains, by carbonate organomineralization of microbial biofilms, or by inorganic mineralization around microbial templates. Here we present a significant discovery that modern thrombolitic microbialites in Lake Clifton, Western Australia, gain their initial structural rigidity from biofilm mineralization by the trioctahedral smectite mineral stevensite. This nucleates in and around microbial filament walls when biological processes suppress carbon and Ca activities, leaving Mg to bind with silica and form a microporous framework that replaces and infills the filament web. After microbial materials are entombed, local carbon and Ca activities rise sufficiently for aragonite microcrystals to grow within the stevensite matrix and perhaps replace it entirely, with eradication of biogenic textural features. This may explain why many ancient microbialite carbonates lack clear evidence for biogenicity. Stevensite may provide the missing link between microbial organomineralization and subsequent abiotic calcification.
    Print ISSN: 0091-7613
    Electronic ISSN: 1943-2682
    Topics: Geosciences
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  • 8
    Publication Date: 2012-12-22
    Description: Cerium L 3 absorption edge ( L 3 -edge) X-ray absorption near edge structure (XANES) spectra were obtained from ~7 x 5 μm areas on green titanite and brown titanite (both with total Ce ~ 0.6 wt%) using the X-ray microprobe at the Pacific Northwest Consortium–X-ray Science Division (PNC-XSD) Insertion Device (ID) line of the Advanced Photon Source (APS). Using a wavelength-dispersive X-ray (WDX) fluorescence detector with a bent LiF (220) crystal monochromator ( E / E ~ 1000), we have overcome the challenge of having to measure trace amounts of Ce in a Ti-rich sample of which the energy of the fluorescence X-rays from Ce L 3 -edge and Ti K -edge excitation cannot be resolved with solid-state detectors. We show that both Ce 3+ and Ce 4+ are present in our titanite samples by examining the Ce L 3 -edge XANES spectra. Our results show that to correctly determine trace element substitution mechanisms in titanite (and other minerals), it is necessary to determine multivalent element concentrations, including Ce 3+ /Ce 4+ . We present a new approach for predicting and evaluating multivalent trace element substitution in titanite and other minerals.
    Print ISSN: 0003-004X
    Electronic ISSN: 1945-3027
    Topics: Geosciences
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  • 9
    Publication Date: 2013-07-02
    Description: Volatile contents of geologic glasses are used to model magma chamber and degassing processes, thus, there is considerable interest in small-scale analytical techniques for analyzing volatiles in glasses. Infrared (IR) spectroscopy has the advantage of determining volatile speciation in glasses (e.g., OH – , molecular H 2 O, molecular CO 2 , and CO 3 2– ). However, sample preparation for the most common IR method used, micro-transmission IR spectroscopy, is complicated because glasses must be prepared as thin, parallel-sided wafers. Raman analysis, while valuable for Fe-poor samples, can be difficult to use for Fe-rich glasses. We have calibrated a micro-reflectance infrared method for determining volatile species using calculated Kramers-Kronig absorbance (KK-Abs.) spectra that requires that only one side of a glass be polished. The method is easier to use than other reflectance methods where it is difficult to determine the baseline for the IR bands. Total H 2 O wt% = m ·(3600 cm –1 KK-Abs.), where m , is the slope of the calibration line that is obtained from a fit to the data. The m value is related to the calculated refractive index, n , for a range of aluminosilicate glass compositions allowing the technique to be applied to samples with unknown calibration slopes. For calc-alkaline andesite glasses we determined calibration slopes for micro-reflectance IR measurements of molecular H 2 O, molecular CO 2 , and CO 3 2– . The method has been calibrated for glasses with up to 6.76 wt% total H 2 O (but is useful for glasses with more than 20 wt% total H 2 O) and has been calibrated for glasses with up to 0.575 wt% total CO 2 . This technique provides a means to analyze volatile abundances in samples that are not possible to analyze or prepare for analysis with transmission micro-IR techniques. We have determined volatile contents in fragile samples such as cracked, vesicular, or crystal-bearing glasses formed by volcanic or impact processes or in high-pressure bubble nucleation experiments and H diffusion experiments. We have monitored H uptake during weathering of basaltic glasses that cannot be polished and determined volatiles in melt inclusions and pumice.
    Print ISSN: 0003-004X
    Electronic ISSN: 1945-3027
    Topics: Geosciences
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  • 10
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