Search results for "Microanalysis"

Rutile crystals as potential trace element and isotope mineral standards for microanalysis

2009

Abstract The present paper reports trace element concentrations of 15 elements (V, Cr, Fe, Zr, Nb, Mo, Sn, Sb, Hf, Ta, W, Lu, Pb, Th and U) as well as Pb and Hf isotope data for four relatively homogeneous and large (centimeter size) rutile grains. Methods employed are SIMS, EMP, LA-ICP-MS, ID-MC-ICP-MS and TIMS. For most elements homogeneity is usually within ± 10% and occasionally variations are even narrower (± 5%), particularly in the core of two of the studied grains. The trace element concentrations of the grains span a broad compositional range (e.g., Zr concentrations are ca. 4, 100, 300 and 800 ppm). Provisional concentration values, calculated based on the homogeneity of the eleme…

Sub 500 nm refractory carbonaceous particles in the polar stratosphere

2017

Abstract. Eleven particle samples collected in the polar stratosphere during SOLVE (SAGE III Ozone loss and validation experiment) from January until March 2000 were characterized in detail by high-resolution transmission and scanning electron microscopy (TEM/SEM) combined with energy-dispersive X-ray microanalysis. A total number of 4175 particles (TEM = 3845; SEM = 330) was analyzed from these samples which were collected mostly inside the polar vortex in the altitude range between 17.3 and 19.9 km. By particle volume, all samples are dominated by volatile particles (ammonium sulfates/hydrogen sulfates). By number, approximately 28–82 % of the particles are refractory carbonaceous with si…

XRMA analysis and X-ray diffraction analysis of dental enamel from human permanent teeth exposed to hydrogen peroxide of varying pH

2019

Background This in vitroinvestigation shows how 3.3% H2O2, at different pH-values affects the enamel. Material and Methods A number of fifteen human premolars were used. The enamel of the coronal half in six of the teeth, were exposed by H2O2. Nine teeth were prepared to enamel powder. The enamel was exposed to 3.3% H2O2, at six different pH-values (pH range 4.5 - 7.0). Analyses of the topography of enamel performed by scanning electron microscope (SEM) and the chemical composition of enamel by X-ray microanalysis (XRMA). X-ray powder diffraction (XRD) analysed the crystallinity in enamel powder. Results The exposure to H2O2 at pH5.5 resulted in a decrease of O in the exposed enamel, and ch…

Scanning Electron Microscopy and X-Ray Microanalysis

2003

Electrochemical analysis of the alterations in copper pigments using charge transfer coefficient/peak potential diagrams. Application to microsamples…

2001

The alteration of copper pigments in art samples was studied by linear scan and cyclic voltammetry using sample-modified Elvacite 2044 film electrodes on the basis of two-dimensional diagrams of charge transfer coefficients calculated from Tafel plots of reductive dissolution processes vs. peak potential. Characteristic voltammetric peaks were obtained for pigments used in the baroque vault frescoes of the Basílica de la Virgen de los Desamparados painted by Antonio Palomino. Results obtained by voltammetric techniques were compared with those from SEM/EDX and FT-IR analysis obtaining a good agreement and leaving to an unambiguous identification of pigments used by Palomino and their altera…

Silica aerogel–metal composites produced by supercritical adsorption

2010

Abstract Silica aerogel has been loaded with ruthenium acetyl acetonate (Ru(acac) 3 ) by adsorption from supercritical carbon dioxide. Adsorption isotherms and kinetics were measured at different pressures and temperatures. The properties of impregnated aerogel were obtained by optical and electron microscopy (SEM), X-ray microanalysis (EDX) and thermogravimetric analysis (TGA). Results showed that Ru(acac) 3 can be uniformly dispersed into the aerogel up to 5 wt%. Moreover, precursor loading is controllable by properly changing operating conditions. The adsorbed metallorganic compound has been reduced to elemental ruthenium by heat treatment without inducing degradation and morphological c…

Microanalysis of the surfaces of natural iron-based minerals by means of synchrotron radiation based experimental techniques

2001

We investigated the surfaces of natural iron-based minerals that are magnetite, hematite, goethite, pyrite, pyrrhotite, chalcopyrite, bornite and vivianite, using synchrotron radiation based techniques. Most iron chalkogenides are very suitable for photoemission microscopy studies due to their low resistivity, which prevents from surface charging. The local compositions were studied employing photoemission microscopy in combination with X-ray absorption spectroscopy. Imaging of the sample in the near-edge region of the absorption edges was used to visualise the spatial distributions of the chemical phases on the surface. Distributions of trace elements are imaged with high chemical and late…

Characterization of prehispanic cosmetics found in a burial of the ancient city of Teotihuacan (Mexico)

2012

The present paper reports the chemical data obtained on samples of pigmenting materials contained in 31 miniature vessels found in a burial found in Teopancazco, a multiethnic neighborhood center located in the southeastern sector of the archaeological site of Teotihuacan (Central Mexico) and the analytical protocol established for the complete characterization of these archaeological materials. For this purpose a multi-technique approach based on the combination of several non destructive and micro-destructive instrumental techniques, namely, light microscopy (LM), scanning electron microscopy-X-ray micro-analysis (SEMe EDX), transmission electron microscopy (TEM), voltammetry of micropart…

FIB-FESEM and EMPA results on Antoninianus silver coins for manufacturing and corrosion processes

2018

[EN] A set of ancient Antoninianus silver coins, dating back between 249 and 274¿A.D. and minted in Rome, Galliae, Orient and Ticinum, have been characterized. We use, for the first time, a combination of nano-invasive (focused ion beam-field emission scanning electron microscopy-X-ray microanalysis (FIB-FESEM-EDX), voltammetry of microparticles (VIMP)) and destructive techniques (scanning electron microscopy (SEM-EDX) and electron microprobe analysis (EMPA)) along with non-invasive, i.e., micro-Raman spectroscopy. The results revealed that, contrary to the extended belief, a complex Ag-Cu-Pb-Sn alloy was used. The use of alloys was common in the flourishing years of the Roman Empire. In th…

Electrochemical identification of flavonoid dyes in solid work of art samples by abrasive voltammetry at paraffin-impregnated graphite electrodes.

2004

Abstract An electrochemical method for identifying flavonoid-type dyes in microsamples from works of art is reported. Square wave voltammograms of natural insoluble dyestuffs based on flavonoid structure dragoon's blood, weld, old fustic, gamboge, Brazilwood and logwood (Campeche wood) attached to paraffin-impregnated graphite electrodes in contact with 0.25 M HAc + 0.25 M NaAc aqueous buffer display characteristic peaks in the potential region between +0.85 and −0.85 V versus AgCl/Ag. Sequential experiments in contact with 0.05 M AlCl 3 and 0.05 M Na 2 MoO 4 plus HAc/NaAc and 0.05 M H 3 BO 3  + 0.10 M NaOH solutions also provide dye-characteristic signals allowing for an unambiguous identi…