Corrosion of silver cones in the subcutaneous connective tissue of the rat: a preliminary scanning electron microscope, electron microprobe, and histological study.
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In the present work a titania network encapsulating a hydroxyapatite particulate phase is proposed as a bioceramic composite coating. The coating on a titanium substrate was produced starting from a sol containing a mixture of titania colloidal particles and hydroxyapatite submicron particles using the dip-coating technique. The microstructure, the morphology and the surface chemical composition of the coating were characterised using X-ray diffraction (XRD), scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS), respectively. Adhesion tests were also performed. These analyses showed that the obtained coating was chemically clean, homogeneous, rough, porous, with a low thickness and well-defined phase composition as well as a good adhesion to the substrate.
X-ray photoelectron spectroscopy (XPS) was measured for the dry body of hydroxyapatite (HAP)-collagen (COL) nanocomposites cross-linked using glutaraldehyde (GA). Survey scan XPS showed the elemental spectra of N, C, O, Ca and P, which came from HAP and COL. The covalent bond formation between Ca2+ of HAP and RCOO- of COL molecule was confirmed by XPS. The bridge formation between COL fibers could be assessed from C1s and N1s band spectrum. The dehydration of swelling water during drying led to the reduction of linking distance for pendant GA between COL fibrils and contributed to further cross-linkage reaction. Cross-linkage induced the enlargement of length scale unit of COL. The modification of length scale was doing the key role of structure manipulation in the cross-linked HAP-COL nanocomposites.
Plasticized poly(vinyl chloride) (PVC) was surface modified by nucleophilic substitution of the chlorine atoms of PVC by thiosulphate in aqueous media in the presence of a phase-transfer catalyst. The properties of the modified surface were evaluated by contact angle measurements, attenuated total reflection Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy and scanning electron microscopy. Migration of the plasticizer di-(2-ethylhexyl) phthalate from control as well as modified PVC was examined in hexane, in cottonseed oil and in poly(ethylene glycol)-400 (PEG-400). While the modified PVC was found to be highly migration resistant in hexane, cottonseed oil and PEG-400 extracted the plasticizer. The modified PVC was found to cause haemolysis and was cytotoxic. A possible explanation for the difference in performance of the modified material in different extraction media and its toxicity is presented from a mechanistic view of the substitution process.
The purpose of this study was to access tissue reactions to the outer prismatic (prism) and the inner nacreous (nacre) layers of the fresh water Margaritifera shell. The materials, in granule form, were implanted into the back muscles and femurs of rats for 1, 2, 4, 8 and 16 weeks. In the back muscles, a foreign body reaction was observed around the implants, starting from one week after implantation and reaching maximal proportions at two weeks. After four weeks, a thin layer of fibrous tissue encapsulated the implanted particles. The external surface of the material stained strongly with acid fuchsin, indicating degradation of implant. At femoral sites, newly formed bone was directly applied to the implant surfaces. The outer-most parts of the organic sheets in prisms were not degraded until 16 weeks after implantation and were embedded in the newly formed bone. The interface between bone and the implants showed close fusion by scanning electron microscopy (SEM). Energy dispersive X-ray analysis (EDAX) demonstrated a phosphorous-rich zone in the interface between bone and the implants, and no electron-dense layer in the interface was found by transmission electron microscopy (TEM). We conclude that Margaritifera shells are biocompatible, biodegradable and osteoconductive materials. Bonding between this natural aragonite and bone seems to occur via a phosphorous-rich intermediate layer.
In the previous paper, boundary conditions matching the probe to the crystal wave function in scanning transmission electron microscopy were applied by matching the whole wave function across the boundary. It is shown here how that approach relates to previous Bloch wave formulations using (phase-linked) plane wave boundary conditions for wave vectors implied by the range of transverse momentum components in the incident probe. Matching the whole wave function across the boundary, and including a suitably fine mesh in the reciprocal space associated with the crystal to allow matching of transverse momentum components within the probe, leads to a structure matrix A containing many elements which would normally be excluded for plane wave incidence. For perfect crystals, the A-matrix may be block diagonalised. This leads to a considerable increase in the computational efficiency of the model and yields important insights into the physics of convergent probes in perfect crystals-reciprocity in coherent imaging and the small aperture limit for coherent and incoherent contrast are considered. The numerical equivalence of the incoherent lattice contrast calculated in this Bloch wave method and the multislice method using mixed dynamic form factors will be demonstrated. Comparison between both these methods and the frozen phonon model, a prevalent multislice method for annular dark field simulation which has the theoretical advantage of handling double channelling, will be made.
Resolution tests on amorphous carbon foils were carried out in an electron microscope with a superconducting system containing 4 lenses including a shielding lens at 200 kV beam voltage. Due to the mechanical and electrical stability of the system and the absence of contamination of the specimen the highest space frequencies transferred at vertically incident beam were 6 nm-1 corresponding to a resolution of 0.17 nm, a value which approaches the theoretical resolving power of the electron optical system. It should also be feasible to apply such a lens system for microprobe analysis without strongly reducing the theoretical resolution limit, if the construction of the shielding lens is slightly changed.
Floating alginate beads have been prepared from alginate solutions containing either dissolved or suspended amoxycillin. The beads were produced by the dropwise addition of the alginate into calcium chloride solution, followed by removal of the gel beads and freeze drying. Drug release studies showed that beads prepared with the drug in solution provided some sustained release characteristics and that these could be improved by the addition of amylose. In all cases, the drug release was consistent with release of a dissolved solute from a granular or porous matrix. The beads retained their buoyancy when amylose and amoxycillin were incorporated, exhibiting resultant weight values greater than zero after 20 h. Preparation of the beads from alginate solutions containing the drug in suspension allowed higher drug loadings, at the expense of faster release and lower buoyancy.
Spherites--round laminated membrane bound structures--are located in the cytoplasm of all cell types of the midgut gland in the harvestmen Gyas annulatus. The spherites consist of an organic matrix composed of glycoproteins and proteoglycans whose sugar portion are carboxylated glycosaminoglycans. Different elements are embedded in this matrix, and their presence varies during the life cycle. All spherites in juveniles are composed of alternating concentrically arranged electron dense and electron lucent layers of organic matrix material before overwintering (December). At that time, spherites contain calcium, phosphorus and silicon. Calcium and phosphorus are located in their electron dense layers, and silicon spotwise, mainly peripheral. Material seems to be lost during overwintering of Gyas as electron lucent "empty" layers appear in spherites in March. The "lost" material could be used as energy supply and/or to provide molecules for synthesis processes during non-nourishing overwintering. Spherites do not contain calcium and phosphorus in July and October. These elements seem to have important biological relevance in the formation and hardening of the cuticle during the moultings in spring. In contrast to calcium and phosphorus, silicon is still stored in spherites in July and October but in decreasing concentration, therefore it could be involved in metabolic processes in adult Gyas. In the period from July to the end of their adult life in late autumn, an increasing number of spherites disintegrate and their remnant organic matrix material progressively aggregates with other cellular waste material in one or more huge vacuoles of glandular cells.
The mechanism of the recrystallization of nano-scale bacterial surface protein layers (S-layers) on solid substrates is of fundamental interest in the understanding and engineering of biomembranes and e.g. biosensors. In this context, the influence of the charging state of the substrate had to be clarified. Therefore, the electrochemical behaviour of the S-layers on gold electrodes has been investigated by in-situ electrochemical quartz microbalance (EQMB) measurements, scanning force microscopy (SFM) and small-spot X-ray photoelectron spectroscopy (SS-XPS) of potentiostatically emersed substrates. It was shown that the negatively charged bonding sites of the S-layer units (e.g. carboxylates) can bond with positively charged Au surface atoms in the positively charged electrochemical double layer region positive of the point of zero charge ( approximately -0.8 V vs. saturated mercury-mercurous sulphate electrode). Surface conditions in other potential regions decelerated the recrystallization and fixation of S-layers. Time-resolved in-situ and ex-situ measurements demonstrated that two-dimensional S-layer crystal formation on gold electrodes can occur within few minutes in contrast to hours common in self-assembled monolayer (SAM) generation. These results proved that the recrystallization and fixation of 2D-crystalline S-layers on an electronic conductor can be influenced and controlled by direct electrochemical manipulation.
The ultrastructural, X-ray microanalytical, histochemical and immunocytochemical features of intraluminal crystalloids found in adenocarcinomas of the parotid gland have been studied. The crystalloids, putatively derived from an abnormal crystalization of salivary duct proteins, are considerably different from the crystalloids found in normal parotid glands, pleomorphic adenomas, and sialocysts.
Besides the use of conventional techniques such as light and polarization microscopy, the present paper proposes the combined use of transmission electron microscopy, secondary and backscattered electron imaging, energy dispersive X-ray analysis and computed tomography for the diagnostic evaluation of ear pathology in the human fetus. These methods were used to revisit the primary calcification front of the fetal otic capsule between 16 and 23 weeks gestational age. Ultramicroscopic evaluation demonstrates similar fetal bone formation to that found in other bones of the human fetus. The formation of the endosteal and periosteal layers is a typical example of early intra-membranous ossification. The enchondral layer is made up of fibrillar bone, laid down around the calcified cartilage remnants. Microchemical analysis indicates a significantly higher Ca/P ratio in the endochondral layer with respect to the endosteum and periosteum. The consequences of a lower Ca/P ratio in the endosteal layer are discussed in view of calcium homeostasis and inner ear function.
The focused ion beam (FIB) tool has been successfully used as both a stand alone analytical instrument and a means to prepare specimens for subsequent analysis by SEM, TEM, SIMS, XPS, and AUGER. In this work, special emphasis is given to TEM specimen preparation by the FIB lift-out technique. The fundamental ion/solid interactions that govern the FIB milling process are examined and discussed with respect to the preparation of electron transparent membranes. TRIM, a Monte Carlo simulation code, is used to physically model variables that influence FIB sputtering behavior. The results of such computer generated models are compared with empirical observations in a number of materials processed with an FEI 611 FIB workstation. The roles of incident ion attack angle, beam current, trench geometry, raster pattern, and target-material-dependent removal rates are considered. These interrelationships are used to explain observed phenomena and predict expected milling behaviors, thus increasing the potential for the FIB to be used more efficiently with reproducible results.
The boundary parameters between contacting spherical bcc-Fe particles have been characterized with the Large Angle Convergent Beam Electron Diffraction (LACBED) technique. The average accuracy of measurements can reach 0.07 degrees. The rotation parameters are interpreted using matrix algebra and evaluated according to the CSL model. The deviation between the experimental results and the reference misorientations given in the CSL model is determined. It is possible to reveal preferential misorientations between irregularly shaped particles with a size less than 100 nm. The method can be applied to nanoparticles and nanocrystalline materials with a wide range of grain orientations, and it is possible to modify it into an automatic method for TEM measurements.
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The bonding of orthodontic brackets to enamel surface using bis-GMA composite resin is usually accomplished by first cleaning the tooth surface then etching with phosphoric acid. This study compared the tensile bond strength of composite resin applied to a tooth surface which had been cleansed with an air-powder polisher to that of the same resin applied to a surface cleansed using a rubber cup and pumice. A wire loop apparatus was attached to bonded orthodontic brackets and pulled in tension in order to test the adherence of the bracket to the tooth. Scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS) were used to evaluate the tooth surface to determine whether sodium bicarbonate material remained after the cleaning operation. All data was analyzed by the one way analysis of variants, the Student-Newman-Keuls test and Duncan's multiple comparison test. No statistical differences were found between the tensile strength of the bonds on the teeth cleansed with the air-powder polisher and those cleansed with a rubber cup and pumice. However, a double exposure of the tooth to phosphoric acid may lower the tensile bond strength by a significant amount.
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