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Results for “Electron Probe Microanalysis”

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PubMed1981

Localization of calcium in an annelid visceral muscle by pyroantimonate deposition and by x-ray microprobe analysis.

The loci of calcium distribution in Nereis pharyngeal visceral muscle have been examined by cytochemical precipitation using potassium pyroantimonate. In Na-, Ca- and Mg-free media, pyroantimonate incubation was used to pinpoint loci of intracellularly bound calcium. This method also revealed heavy deposition on the inner face of the plasma membrane, in the sarcoplasmic reticulum and nucleus. X-ray microprobe analysis of the precipitate confirmed the presence of calcium and antimony peaks. It is concluded that the plasma membrane may constitute a major calcium pool for the activation of contraction in this muscle.

Animals↗
PubMed1984

Comparison of surface layer properties of composite resins by ESCA, SEM and X-ray diffractometry.

Hyperfine surface layer properties of three types of dental composite resins, highly-filled, conventional, and micro-filled resins, were studied using X-ray photoelectron spectroscopy (ESCA) by a combination of X-ray diffractometry and scanning electron microscopy (SEM). X-ray diffraction and SEM analysis showed clearly that each resin has different characteristics of SiO2 particle size and distribution. ESCA depth resolution with argon ion etching indicated that, in contrast to conventional and microfilled resins, carbon due to polymers of highly-filled resin decreases dramatically with increasing depth in the nanometer range of the resin-rich surface layer.

Composite Resins↗
PubMed1994

Characterization of calcium phosphate powders by ESCA and EDXA.

Calcium phosphate (CaP) materials can be well characterized by traditional methods such as wet chemistry and X-ray diffraction (XRD). These methods, however, offer limitations when non-destructive evaluation of CaP coatings on curved surfaces is required. Since the source powders for these coatings are generally commercially available CaP powders, careful characterization of the source powders may allow inferences to be made regarding the effects of plasma spraying on coating composition. Nine commercially available CaP powders were characterized by scanning electron microscopy, wet chemistry and XRD. These techniques showed that major differences exist between individual powders claiming to be hydroxyapatite. Analysis of these nine powders by electron spectroscopy for chemical analysis (ESCA) and energy dispersive X-ray analysis (EDXA) suggest that these techniques can provide the chemical composition of CaP in a non-destructive manner and thus may be of use in determining the composition of CaP in configurations (such as coatings on metal surfaces) not readily amenable to traditional methods. A calibration curve is required, however, to relate this surface chemical composition result to the material's bulk composition as determined by wet chemistry analysis. Errors of less than 10% can be obtained using ESCA and EDXA. These studies suggest that non-destructive chemical composition evaluation by EDXA and ESCA may also be applicable to CaP coatings.

Calcium Phosphates↗
PubMed1994

In vitro exposure of a novel polyesterurethane graft to enzymes: a study of the biostability of the Vascugraft arterial prosthesis.

The biostability of the Vascugraft arterial prosthesis, a porous synthetic graft made by a novel spinning process from a unique poly(ester urethane) polymer, has been studied by means of an in vitro enzyme incubation technique. Samples of the Vascugraft were exposed to buffered solutions of collagenase and pancreatin, as well as the buffer solutions alone, for periods of up to 100 days at 37 +/- 1 degrees C. On removal and after cleaning, a number of different analytic methods, including X-ray photoelectron spectroscopy for chemical analysis (ESCA), attenuated total reflectance-Fourier transform infrared spectroscopy (ATR-FTIR), differential scanning calorimetry (DSC), size exclusion chromatography (SEC), scanning electron microscopy (SEM), interference microscopy, moisture content and contact angle measurements, were used to examine the changes in chemical structure and surface morphology of the samples. During incubation in both enzymes the molecular weight of the polyurethane appeared to decrease in the presence of enzyme but increase in the presence of buffer. Further microphase separation in the polyurethane material developed during incubation in buffer solutions. Such changes in microstructure were associated with increased surface hydrophilicity, increased moisture content and a significant improvement in the extent of order and preferred orientation of the hard segment domains within the fibres. In the sampling depth of about 5 nm, both enzymes decreased the carbonate group content at the surface of the prosthesis to as little as 40% of their original values. The results from ATR-FTIR and DSC demonstrated that this phenomenon was limited primarily to the soft segment phase. While the Vascugraft prosthesis did exhibit some limited chemical modifications on exposure to concentrated enzyme solutions, nevertheless such changes were confined to the surface layer of the polyurethane microfibres. The importance and significance of those results will be more adequately determined by in vivo investigation.

Blood Vessel Prosthesis↗
PubMed1983

X-ray microscopy using a scanning electron microscope for the purpose of imaging central nervous system structures.

A simple modification of an Hitachi S.450 specimen stage permits point source X-ray microscopy with a scanning electron microscope. Point source X-ray microscopy was applied to nervous tissue to determine the feasibility of utilizing this technique instead of a light microscope mounted camera lucida to produce 2- and 3-dimensional images of whole structures such as neurons. Various target materials, radio-opaque materials and photographic films were examined in this study.

Animals↗
PubMed1987

Characterization of electrode dissolution products on the high-voltage electron microscope.

Deposits left by electrodes and biocompatibility test specimens implanted in brain or peripheral nerve were characterized by X-ray microprobe analysis, electron diffraction and stereoscopic imaging using a high-voltage electron microscope. Examination of thick (1-micron) sections of neural tissue confirmed that the electron-dense bodies found adjacent to electrode positions consist of elements originating in the implant material (with the exceptions of the S and Se found in association with Ag). These elements have no long-range order, suggesting they are complexed with biological molecules. In some cases the deposits appear to be caused by pulsing the electrode with current, while in other cases the deposits are corroded or abraded from the electrode or are otherwise not associated with the neuroprosthetic functioning of the implant.

Animals↗
PubMedDate not supplied

Contribution of electron energy loss spectroscopy to the development of analytical electron microscopy.

The combined use of an electron energy loss spectrometer and an electron microscope provides some chemical information at the nanometer scale. The physics of the interaction processes between the incident electron beam and the thin sample foil is reviewed in terms of energy and momentum transfer. This analysis of the content of an electron energy loss spectrum allows us to establish rules for a satisfactory use of the information and to discuss the detection limits of this newly developed microanalytical technique.

Electron Probe Microanalysis↗
PubMed1988

Electron spectroscopic imaging of DNA.

Electron spectroscopic imaging (ESI) was carried out using a fixed beam electron microscope equipped with a parallel electron energy filter to form micrographs of purified plasmid DNA without the use of heavy metal stains and shadows. Inelastically scattered electrons that have ionized the phosphorus LII,III shell electrons were used to form phosphorus distribution maps of DNA and deoxyribonucleoprotein complexes. Signal-to-noise values of the net phosphorus content over single DNA molecules compared to two and four interwound DNA strands directly reflect the known stoichiometric levels of phosphorus content, illustrating that ESI can be used to determine the relative levels of nucleic acid in nucleoprotein complexes. An initial attempt to characterize nucleosomal and transcriptionally active chromatin from Saccharomyces cerevisiae with this technique reveals three distinct ultrastructural classes of the basic chromatin fiber.

DNA↗
PubMed1988

Phosphorus imaging of the 7-S ribonucleoprotein particle.

In this study an unprecedented demonstration of the detection sensitivity of electron spectroscopic imaging (ESI) is reported. This microanalytical technique is capable of forming elemental maps of a specimen with high sensitivity and resolution by forming images with electrons that have lost particular amounts of energy due to interactions with the atoms of the specimen. The 7-S ribonucleoprotein particle, composed of one molecule of 5-S RNA and one molecule of the 40K MW protein, TFIIIa, was used for this demonstration. As few as 120 phosphorus atoms of the 5-S RNA have been detected and their localization in the particle determined. The shape of the 7-S particle is ellipsoidal with a long axis of 15.0 nm and a shorter axis between 8 and 9 nm. Similarly, the 5-S RNA is also an elongated structure located asymmetrically on one side of the particle. The average signal-to-noise ratio over the particle in the net phosphorus images is 14 whereas the ratio measured for the nucleosome containing 2.4-fold more phosphorus is 30.

Animals↗
PubMed1988

Ultrastructural analysis of bone nodules formed in vitro by isolated fetal rat calvaria cells.

When cells enzymatically digested from 21 d fetal rat calvaria are grown in ascorbic acid and Na beta-glycerophosphate, they form discrete three-dimensional nodular structures with the histological and immunohistochemical appearance of woven bone. The present investigation was undertaken to verify that bone-like features were identifiable at the ultrastructural level. The nodules formed on top of a fibroblast-like multilayer of cells. The upper surface of the nodules was lined by a continuous layer of cuboidal osteoblastic cells often seen to be joined by adherens junctions. Numerous microvilli, membrane protrusions, and coated pits could be seen on the upper surface of these cells, their cytoplasm contained prominent RER and Golgi membranes, and processes extended from their lower surfaces into a dense, highly organized collagenous matrix. Some osteocyte-like cells were completely embedded within this matrix; they also displayed RER and prominent processes which extended through the matrix and often made both adherens and gap junctional contacts with the processes of other cells. The fibroblastic cells not participating in nodule formation were surrounded by a less dense collagenous matrix and, in contrast to the matrix of the nodules, it did not mineralize. An unmineralized osteoid-like layer was seen directly below the cuboidal top layer of cells. A mineralization front was detectable below this in which small, discrete structures resembling matrix vesicles and feathery mineral crystals were evident and frequently associated with the collagen fibrils. More heavily mineralized areas were seen further into the nodule. Electron microprobe and electron and X-ray diffraction analysis confirmed the mineral to be hydroxyapatite.(ABSTRACT TRUNCATED AT 250 WORDS)

Animals↗
PubMed2004

Raman microscopy of selected tungstate minerals.

A series of tungstate bearing minerals including scheelite, stolzite, ferberite, hübnerite, wolframite, russellite, tungstenian wulfenite and cuprotungstite have been analyzed by Raman microscopy. The results of the Raman spectroscopic analysis are compared with published data. These minerals are closely related and often have related paragenesis. Raman microscopy enables the selection of individual crystals of these minerals for spectroscopic analysis even though several of the minerals can be found in the same matrix because of the pargenetic relationships between the minerals. The Raman spectra are assigned according to factor group analysis and related to the structure of the minerals. These minerals have characteristically different Raman spectra. The nu1(Ag) band is observed at 909 cm(-1) and although the corresponding nu1(Bu) vibration should be inactive a minor band is observed around 894 cm(-1). The bands at 790 and 881 cm(-1) are associated with the antisymmetric and symmetric Ag modes of terminal WO2. The band at 695 cm(-1) is interpreted as an antisymmetric bridging mode associated with the tungstate chain. The nu4(Eg) band was absent for scheelite. The bands at 353 and 401 cm(-1) are assigned as either deformation modes or as r(Bg) and delta(Ag) modes of terminal WO2. The band at 462 cm(-1) has an equivalent band in the infrared at 455 cm(-1) assigned as delta(as)(Au) of the (W2O4)n chain. The band at 508 cm(-1) is assigned as nu(sym)(Bg) of the (W2O4)n chain.

Electron Probe Microanalysis↗
PubMed2006

Raman spectroscopic study of the molecular structure of the uranyl mineral zippeite from Jáchymov (Joachimsthal), Czech Republic.

Raman spectra at 298 and 77K and infrared spectra of the uranyl sulfate mineral zippeite from Jáchymov (Joachimsthal), Czech Republic, K(0.6)(H(3)O)0.4[(UO(2))6(SO(4))3(OH)7].8H2O, were studied. Observed bands were tentatively attributed to the (UO(2))2+ and (SO(4))2- stretching and bending vibrations, the OH stretching vibrations of water molecules, hydroxyls and oxonium ions, and H(2)O, oxonium, and delta U-OH bending vibrations. Empirical relations were used for the calculation of U-O bond lengths in uranyl R (A)=f(nu(3) or nu(1)(UO(2))2+). Calculated U-O bond lengths are in agreement with U-O bond lengths from the single crystal structure analysis and those inferred for uranyl anion sheet topology of uranyl pentagonal dipyramidal coordination polyhedra. The number of observed bands supports the conclusion from single crystal structure analysis that at least two symmetrically distinct U6+ (in uranyls) and S6+ (in sulfates), water molecules and hydroxyls may be present in the crystal structure of the zippeite studied. Strong to very weak hydrogen bonds present in the crystal structure of zippeite studied were inferred from the IR spectra.

Czech Republic↗
PubMed2002

Characterisation of cement pastes by inverse gas chromatography.

Two cement pastes, commonly used in concrete formulations, were characterised by IGC at 35-80 degrees C before and after coating with an epoxy resin and a hardener. The cements are mixtures of hydrates in various proportions, such as calcium silicate hydrate (CaO-SiO2-H2O) and calcium hydroxide Ca(OH)2. Apolar and polar probes were used to determine the dispersive and acid-base characteristics of the cement pastes. These materials have high surface energy as judged from the dispersive contribution to the surface free energy (gamma(s)d) values lying in the 50-70 mJ/m2 range at 60-80 degrees C. Examination of the specific interactions permitted to show that the cement pastes are strongly amphoteric species with a substantial predominant Lewis basicity that is in line with the basic pH of their aqueous suspensions. Following coating with an epoxy resin (DGEBA) and a hardener (triethylene tetramine), the surface energy of the cements decreases substantially with the mass loading of the organic material. The surface thermodynamic properties were also correlated with the surface chemical composition as determined by X-ray photoelectron spectroscopy.

Chromatography, Gas↗