Energy-dispersive X-ray Spectroscopy for the Quantitative Analysis of Pyrite Thin Specimens

To explore ways to improve the accuracy of quantitative analysis of samples in the micrometer to nanometer range of magnitudes,we adopted analytical transmission electron microscopy(AEM/EDS)for qualitative and quantitative analysis of pyrite materials.Additionally,the k factor of pyrite is calculated experimentally.To develop an appropriate non-standard quantitative analysis model for pyrite materials,the experimentally calculated k factor is compared with that estimated from the non-standard quantitative analytical model of the instrument software.The experimental findings demonstrate that the EDS attached to a TEM can be employed for precise quantitative analysis of micro-and nanoscale regions of pyrite materials.Furthermore,it serves as a reference for improving the results of the EDS quantitative analysis of other sulfides.

Use of near-infrared reflectance spectroscopy for the rapid determination of the digestible energy and metabolizable energy content of corn fed to growing pigs

Background： The ability of near-infrared reflectance spectroscopy（NIRS） to determine the digestible energy（DE）and metabolizable energy（ME） content of corn fed to growing pigs was tested. One hundred and seventeen corn samples, comprising different planting regions and varieties were collected from all over China in a three-year period. The samples were randomly split into a calibration set（n = 88） and a validation set（n = 29）. The actual and calculated DE and ME content of the corn samples was determined by digestion-metabolism experiments and the prediction equations of Noblet and Perez（J Anim Sci. 71：3389–98,1993）. The samples were then subjected to NIRS scanning and calibrations were performed by the modified partial least square（MPLS） regression method based on77 different spectral pre-treatments. The NIRS equations based on the actually determined and calculated DE and ME were built separately and then validated using validation samples.Results： The NIRS equations obtained from actually determined DE, the coefficient of determination for calibration（RSQcal）, cross-validation（R^2CV）, and validation（RSQv） were 0.89, 0.87 and 0.86, and these values for determined ME were 0.87, 0.86 and 0.86. For the NIRS equations built from calculated DE, the RSQcal, R^2CV, and RSQvvalues were 0.88, 0.85 and 0.84, and these values for calculated ME were 0.86, 0.84 and 0.82. Except for the equation based on calculated ME（RPD_v= 2.38, 〈 2.50）, the other three equations built from actually determined energy and calculated DE produced good prediction performance（RPD_vranging from 2.53 to 2.69, 〉 2.50） when applied to validation samples.Conclusion： These results indicate that NIRS can be used as a quantitative method for the rapid determination of the available energy in corn fed to growing pigs, and the NIRS equations based on the actually determined energy produced better predictive performance than those built from calculated energy values.

Energy Dispersive X-Ray Spectroscopy of the Sohnari Member of Laki Formation from Southern Indus Basin of Pakistan

This study determines the geochemical and depositional environment analysis of the sediments of the Sohnari Member of the Laki Formation, Northern Kirthar Fold Belt of Pakistan. The Energy-Dispersive-X-Ray Spectroscopy (EDS) technique is used for the detection of major elements and the effects of shifting depositional climatic conditions of six representative samples which were acquired from the Sohnari Member of the Laki Formation at Lakhra area, Sindh, Pakistan. The sedimentological studies clarify that the sediments the Sonahri Member are relatively immature and most migrated in clastic mode. The availability of Silica shows that the Member was formed due to biochemical precipitation and detrital mode and was deposited at a fast rate of sediment deposition under the fluvio-deltaic depositional system. This is also deduced that the rapid rate of sediment deposition might be created a reducing atmosphere and allowing for the mineralization of sulphur.

Gap States of ZnO Thin Films by New Methods:Optical Spectroscopy,Optical Conductivity and Optical Dispersion Energy

The optical reflectance and transmittance spectra in the wavelength range of 300-2500 nm are used to compute the absorption coefficient of zinc oxide films annealed at different post-annealing temperatures 400, 500 and 600°C.The values of the cross point between the curves of the real and imaginary parts of the optical conductivity ɑ_1 and ɑ_1 with energy axis of films exhibit values that correspond to optical gaps and are about 3.25-3.3 eV. The maxima of peaks in plots dR/dλ and dT/dλ versus wavelength of films exhibit optical gaps at about 3.12-3.25 eV.The values of the fundamental indirect band gap obtained from the Tauc model are at about 3.14-3.2 eV. It can be seen that films annealed at 600°C have the minimum indirect optical band gap at about 3.15 eV. The films annealed at 600°C have Urbach＇s energy minimum of 1.38 eV and hence have minimum disorder. The dispersion energy d of films annealed at 500°C has the minimum value of 43 eV.

Temperature Evolution of Energy Gap and Band Structure in the Superconducting and Pseudogap States of Bi_2Sr_2CaCu_2O_(8＋δ) Superconductor Revealed by Laser-Based Angle-Resolved Photoemission Spectroscopy

We carry out detailed momentum-dependent and temperature-dependent measurements on Bi_2Sr_2CaCu_2O_（8＋δ）（Bi2212） superconductor in the superconducting and pseudogap states by super-high resolution laser-based angleresolved photoemission spectroscopy. The precise determination of the superconducting gap for the nearly optimally doped Bi2212（T_c= 91 K） at low temperature indicates that the momentum-dependence of the superconducting gap deviates from the standard d-wave form（cos（2Φ））. It can be alternatively fitted by including a high-order term（cos（6Φ）） in which the next nearest-neighbor interaction is considered. We find that the band structure near the antinodal region smoothly evolves across the pseudogap temperature without a signature of band reorganization which is distinct from that found in Bi_2Sr_2CuO_（6＋δ） superconductors. This indicates that the band reorganization across the pseudogap temperature is not a universal behavior in cuprate superconductors.These results provide new insights in understanding the nature of the superconducting gap and pseudogap in high-temperature cuprate superconductors.

A double toroidal analyzer for scanning probe electron energy spectrometer

An ultra-high vacuum （UHV） compatible electron spectrometer employing a double toroidal analyzer has been de- veloped. It is designed to be combined with a custom-made scanning tunneling microscope （STM） to study the spatially localized electron energy spectrum on a surface. A tip-sample system composed of a piezo-driven field-emission tungsten tip and a sample of highly ordered pyrolytic graphite （HOPG） is employed to test the performance of the spectrometer. Two-dimensional images of the energy-resolved and angle-dispersed electrons backscattered from the surface of HOPG are obtained, the performance is optimized and the spectrometer is calibrated. A complete electron energy loss spectrum covering the elastic peak to the secondary electron peaks for the HOPG surface, acquired at a tip voltage of -140 V and a sample current of 0.5 pA, is presented, demonstrating the viability of the spectrometer.

Possible Relevance of the Allende Meteorite Conditions in Prebiotic Chemistry: An Insight into the Chondrules and Organic Compounds

The study of the mineral and organic content of the Allende meteorite is important for our understanding of the molecular evolution of the universe as well as the ancient Earth. Previous studies have characterized the magnetic minerals present in ordinary and carbonaceous chondrites, providing information on the evolution of magnetic fields. The interaction of organic compounds with magnetic minerals is a possible source of chemical diversity, which is crucial for molecular evolution. Carbon compounds in meteorites are of great scientific interest for a variety of reasons, such as their relevance to the origins of chirality in living organisms. This study presents the characterization of organic and mineral compounds in the Allende meteorite. The structural and physicochemical characterization of the Allende meteorite was accomplished through light microscopy, powder X-ray diffraction with complementary Rietveld refinement, Raman and infrared spectroscopy, mass spectrometry, scanning electron microscopy, and atomic force microscopy using magnetic signal methods to determine the complex structure and the interaction of organic compounds with magnetic Ni-Fe minerals. The presence of Liesegang-like patterns of chondrules in fragments of the Allende structure may also be relevant to understanding how the meteorite was formed. Other observations include the presence of magnetic materials and nanorod-like solids with relatively similar sizes as well as the heterogeneous distribution of carbon in chondrules. Signals observed in the Raman and infrared spectra resemble organic compounds such as carbon nanotubes and peptide-like molecules that have been previously reported in other meteorites, making the Mexican Allende meteorite a feasible sample for the study of the early Earth and exoplanetary bodies.

Study on Physical Process of Surface Oxidation of Rare Earth-Transition Metal Amorphous Magneto-Optical Thin Films

By using surface effects(Auger electron spectroscopy,X-ray photoelectron spectroscopy,polar Kerr effect)and volume effects(magnetization,torque curve)the physical process of surface oxidation of rare earth-transition metal amorphous magneto-optical thin films was studied in this paper.The rare earth elements oxidize preferentially and rich at the film surface,and the transition metals deplete in oxidation layer.Fe_2O_3 in the surface oxidation layer contributes to the planar magnetization,and thereby the anomalous peak appears near 180° on the torque curves and the amplitude of the peaks is related to the depth of surface oxidation layers.The iron bonds to oxygen easier than the cobolt.RE-Co magneto-optieal thin films have good properties of resistance to oxidation and humidity.

New approaches to characterizing urban air particles in central London

Atmospheric particles in central London during July 1996 have been apportioned to sources by two complimentary techniques: (1) morphological characteristics, determined using high power light microscopy; (2) chemical composition determined by energy dispersive spectroscopy. During the study period, the majority of particles were found to be either biological in origin, or from vehicle related combustion processes. Trends in the latter group of particles are explored further. Numbers of particles per cubic metre were determined at an hourly resolution over a period of six days, and were found to be significantly correlated with other traffic pollutants such as benzene and 1,3 butadiene, although there is no relationship with mass of PM10 as measured by a nearby UK Government monitoring station. We suggest in this paper that numbers of particles from car exhausts are more representative of traffic pollution than current estimates which use monitoring by mass.

Three-dimensional size and orientation of the precipitates in AZ91 magnesium alloys measured by TEM techniques

Knowledge of the microscopic structure, including three-dimensional （3-D） size and orientation of the precipitates, is essential to fully understand the mechanical properties of the magnesium alloys and designing the alloys with better performance. Analytical TEM with high spatial resolution offers the simultaneous measurements of 3-D size, structure, orientation, composition of the precipitates from one typical sample along an established crystallographic axis. Besides popular Burgers orientation relationship （OR）, other ORs such as Pitsch-Schrader OR, Crawley OR, Potter OR and a new OR with the form of [0001]α 1.0° from [311]γ and （1120）α 2.0° from （033）γ between the magnesium matrix and the precipitate γ-MglTAl 12 are identified by TEM imaging and diffraction techniques. As a case study, the thicknesses of the individual precipitates with Burgers OR are further measured to be 100 200 nm through both electron energy-loss spectroscopy and x-ray energy dispersive spectroscopy combining differential x-ray absorption and extrapolation, which are in agreement with the overall 3-D size statistic distribution results obtained through analysing various samples along various directions. Furthermore, the fabricated wedge-shape structure provides a platform on which to study the dependence of the interfacial strain on the variation of the thickness.

Determination of Water Diffusion Coefficients and Dynamics in Adhesive/Carbon Fiber Reinforced Epoxy Resin Composite Joints

To determinate the water diffusion coefficients and dynamics in adhesive/carben fiber reinforced epoxy resin composite joints, energy dispersive X-ray spectroscopy analysis（EDX） is used to establish the content change of oxy- gen in the adhesive in adhesive/carbon fther reinforced epoxy resin composite joints. As water is made up of oxygen and hydrogen, the water diffusion coefficients and dynamics in adhesive/carben fiber reinforced epoxy resin composite joints can be obtained from the change in the content of oxygen in the adhesive during humidity aging, via EDX analy-sis. The authors have calculated the water diffusion coefficients and dynamics in the adhesive/carbon fiber reinforced epoxy resin composite joints with the aid of beth energy dispersive X-ray spectroscopy and elemental analysis. The de- termined results with EDX analysis are almost the same as those determined with elemental analysis and the results al- so show that the durability of the adhesive/carbon fther reinforced epoxy resin composite joints subjected to silane cou- pling agent treatment is better than those subjected to sand paper burnishing treatment and chemical oxidation treat- ment.

Impact of open dumping of municipal solid waste on soil properties in mountainous region

This paper presents the effect of open dumping of municipal solid waste(MSW) on soil characteristics in the mountainous region of Himachal Pradesh, India. The solid waste of dumpsite contains various complex characteristics with organic fractions of the highest proportions. As leachate percolates into the soil, it migrates contaminants into the soil and affects soil stability and strength. The study includes the geotechnical investigation of dump soil characteristics and its comparison with the natural soil samples taken from outside the proximity of dumpsites. The geochemical analysis of dumpsite soil samples was also carried out by scanning electron microscopy(SEM) and energy dispersive X-ray spectroscopy(EDS).Visual inspection revealed that the MSW consists of high fraction of organics, followed by paper. The soil samples were collected from five trial pits in the dumpsites at depths of 0.5 m, 1 m and 1.5 m. Then the collected soil samples were subjected to specific gravity test, grain size analysis, Atterberg’s limit test,compaction test, direct shear test, California bearing ratio(CBR) test and permeability analysis. The study indicated that the dumpsite soils from four study regions show decreasing trends in the values of maximum dry density(MDD), specific gravity, cohesion and CBR, and increasing permeability as compared to the natural soil. The results show that the geotechnical properties of the soils at all four study locations have been severely hampered due to contamination induced by open dumping of waste.

Effect of liner and porcelain application on zirconia surface structure and composition

The purpose of this study was to determine if there is an effect of liner and porcelain application （layering and pressing techniques） on the surface of yttria-stabilized tetragonal zirconia polycrystals （Y-TZP）, which were exposed to permutations of liner, layered porcelain, and pressed porcelain. Scanning electron microscope （SEM）/energy dispersive spectroscope （EDS） was used to identify changes in composition and microstructure after removing liner and porcelain with hydrofluoric acid. Simulated aging was also conducted to determine the effect of liner and porcelain on low-temperature degradation. The control group had a typical equiaxed grain structure, referred to as unaffected. When covered with liner or porcelain, some areas changed in structure and composition and were termed affected. The frequency of affected sbructure decreased when liner was covered with either layered porcelain or pressed porcelain. There were statistical differences （P〈0.05） in the composition between affected and unaffected for zirconium （layered porcelain with liner： affected = 60% （0.8%） （m/m）, unaffected = 69% （4%）, layered porcelain without liner： affected = 59% （3%）, unaffected = 65% （3%）） and oxygen （layered porcelain with liner： affected = 35% （2%）, unaffected = 26% （4%）, layered porcelain without liner： affected = 35% （3%）, unaffected = 30% （2%））. However, there were statistical differences （P〈0.05） in the composition for zirconium and oxygen of the aged layered porcelain without liner only. The liner should not be used before porcelain application, especially when using the layering technique for zirconia restorations. Furthermore, pressing should be considered the technique of choice over layering.

Palaeodiet of Miocene Producers and Depositional Environments:Inferences from the First Evidence of Microcoprolites from India

This paper reviews research on coprolites from India,providing the first evidence of microcoprolites from the early Miocene(Aquitanian)Khari Nadi Formation sedimentary succession,exposed about 1.5 km northeast of the village of Kotada,Kachchh(Kutch)District,Gujarat State,western India.Morphometric and size comparisons(in a statistical framework)with known coprolites from the Mesozoic-Cenozoic successions of India(including those recorded herein)and globally suggest that fishes were the likely producers of the Kotada coprolites.Scanning electron microscopy confirms the presence of fish dental remains within the coprolites,while both Scanning Electron Microscopy(SEM)and Energy Dispersive X-ray Spectroscopy(EDS)reveal the phosphatic nature of the microscopic coprolite specimens(recorded herein)hinting that the producer(s)were predominantly carnivorous(ichthyophagous)in their diet.Furthermore,X-Ray Fluorescence(XRF)analysis of the host and associated lithologies allows us to deduce that the Kotada coprolites were deposited in a shallow marine environment,with possible aerial exposure of the host lithology occurring at some point after deposition.To the best of our knowledge,the present report is the first record of microscopic fish coprolites from India,as well as being the first from the Aquitanian of India and the oldest Neogene record from India.

Collective excitations and quantum size effects on the surfaces of Pb(111)films:An experimental study

Pb(111)film is a special system that exhibits strong quantum size effects in many electronic properties.The collective excitations,i.e.,plasmons,in Pb(111)films are also expected to show signatures of the quantum size effect.Here,using high-resolution electron energy loss spectroscopy,we measured the plasmons on the surface of Pb(111)films with different film thicknesses and analyzed the plasmon dispersions.One surface plasmon branch exhibits prominent damping in the small momentum range,which can be attributed to the interaction between the top and bottom interfaces of the Pb(111)films.With the film thickness increasing,the critical momentum characterizing the damping in Pb(111)films decays not only much slower in Pb(111)films than in other metal films,and even in films with the thickness up to 40 monolayers the damping still exists.The slow decay of the surface plasmon damping,manifesting the strong quantum size effect in Pb(111)films,might be related to the strong nesting of the Fermi surface along the(111)direction.

Design of a novel correlative reflection electron microscope for in-situ real-time chemical analysis

A novel instrument that integrates reflection high energy electron diffraction(RHEED),electron energy loss spectroscopy(EELS),and imaging is designed and simulated.Since it can correlate the structural,elemental,and spatial information of the same surface region via the simultaneously acquired patterns of RHEED,EELS,and energy-filtered electron microscopy,it is named correlative reflection electron microscopy(c-REM).Our simulation demonstrates that the spatial resolution of this c-REM is lower than 50 nm,which meets the requirements for in-situ monitoring the structural and chemical evolution of surface in advanced material.

Spatially Resolved Analytical Electron Microscopy at Grain Boundaries of α-Al_2O_3

In this work the electronic structure and the impurity excess of the basal and rhombohedral twin grain boundaries are investigated, using electron energy loss spectroscopy (EELS) and energy dispersive X-ray spectroscopy (EDXS). The measurability of electronic structures of the twin grain boundaries are discussed by comparing theoretical density of states (DOS) from bulk material with interfacial DOS, obtained from local density functional theory (LDFT) calculations.

Highly efficient and stable electrooxidation of methanol and ethanol on 3D Pt catalyst by thermal decomposition of In2O3 nanoshells

In this paper In2O3nanoshells have been synthesized via a facile hydrothermal approach. The nanoshells can be completely cracked into pony-size nanocubes by annealing, which are then used as a support of Pt catalyst for methanol and ethanol electrocatalytic oxidation. The prepared In2O3and supported Pt catalysts (Pt/In2O3) were characterized by X-ray diffraction (XRD), energy dispersive X-ray spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS), field effect scanning electron microscopy (FESEM), and transmission electron microscopy (TEM). Cyclic voltammetry (CV), linear sweep voltammetry (LSV), chronoamperometry and electrochemical impedance spectroscopy (EIS) were carried out, indicating the excellent catalytic performance for alcohol electrooxidation can be achieved on Pt/In2O3nanocatalysts due to the multiple active sites, high conductivity and a mass of microchannels and micropores for reactant diffusions arising from 3D frame structures compared with that on the Pt/C catalysts. © 2016 Science Press

Analytical potential energy function and spectroscopy parameters for B^1Π state of KH

Multi-reference configuration interaction is used to produce potential energy curves （PECs） for the excited B1FI state of KH molecule. To investigate the correlation effect of core-valence electrons, five schemes are employed which include the different correlated electrons and different active spaces. The PECs are fitted into analytical potential energy functions （APEFs）. The spectroscopic parameters, ro-vibrational levels, and transition frequencies are determined based on the APEFs and compared with available experimental and theoretical data. The molecular properties for B1II obtained in this letter, which are better than those available in literature, can be reproduced with calculations using the suitable correlated electrons and active space of orbitals.

X-Ray and Mössbauer Study of Magnetic Black Sand from Mayotte Island

Natural magnetic black sands are known from several sites often located in areas of volcanic origin. Their elemental and mineral composition provides information on the geology of their territory and depends on several factors occurred during their formation. A sample of black sand was collected on the seashore of the island of Mayotte in the Indian Ocean and its magnetic part was investigated by means of energy dispersive X-ray spectroscopy (EDS), powder X-ray diffraction (XRD), and MÖssbauer spectroscopy at room temperature. The mineral composition is dominantly magnetite, in good agreement with samples collected in other sites of volcanic origin. Contrary to pure magnetite, a relevant fraction of Ti was detected by EDS. The 16% Ti and 1% Mn content increase the magnetite lattice parameter to 8.4312 (25) Å. The broadening of XRD lines pointed towards a significant degree of disorder. This was confirmed by MÖssbauer spectroscopy and is attributed to the presence of Ti replacing Fe in the magnetite lattice. The presence of Ti modifies the local magnetic field on the Fe sites, leading to a broader and more complex MÖssbauer transmission spectrum with respect to the one of pure magnetite. To study the effect of temperature, samples were heated for 12 hours to 600°C and 800°C in argon and to 1000°C in air. Annealing in argon did not improve the crystallinity while annealing in air caused a complete decomposition of magnetite into hematite and pseudobrookite.