Suggestions for the quantitative X-ray microanalysis of thin sections of frozen-dried and embedded biological tissues

When a microregion in a thin section of frozen-dried and embedded tissue is analysed by the conventional electron-probe X-ray continuum-normalization method, the measured quantity is in mmol of element per kg of embedded specimen. As each microregion contains an unknown amount of embedding medium, this quantity generally lies indeterminately somewhere within the wide range between mmol of element per kg of hydrated tissue and mmol of element per kg of dehydrated tissue. However, if a ‘tag’ element is incorporated in the embedding medium, the contribution of the medium to the local continuum count in each probed field should be measurable, and the X-ray data may then unambiguously yield mmol of element per kg of dehydrated tissue. This result should not be affected by shrinkage on freeze-drying or by incomplete replacement of water by embedding medium. The same X-ray data can additionally provide estimates of mmol of element per unit volume, mmol of element per kg of hydrated tissue and local dry-mass fraction. However, these estimates are subject to errors due to tissue shrinkage, incomplete replacement of water and beam damage.     

Formation of layered structure on bismuth-borate glass surface

X-ray diffraction analysis shows that the transformation during heat treatment from amorphous to crystalline phases of bismuth-borate glass samples takes place in sequences. After a short heat treatment, 5 min at 550 °C, a layered structure with a preferred orientation of crystallites on the surface is observed. After a long heat treatment, 8 h at the same temperature, normal polycrystalline bulk samples are obtained.     

A versatile data acquisition system for time resolved X-ray scattering using gas proportional detectors with delay line readout

A data acquisition system for time resolved X-ray scattering experiments using linear, quadrant or area gas proportional detectors with delay line readout based on commercially available hardware (National Instruments) is described. The system can easily be configured for recording data from point detectors (e.g. photomultipliers and photodiodes) and/or ancillary data only. Applications involving measurements with two different types of time to digital converters illustrate the features and performances of the system.     

Acidity and basicity of hydrotalcite derived mixed Mg-Al oxides studied by test reaction of MBOH conversion and temperature programmed desorption of NH3 and CO2

Mg-Al hydrotalcites intercalated with five different interlayer anions—CO₃²⁻, SO₄²⁻, Cl⁻, HPO₄²⁻ or terephthalate—were synthesized by either the coprecipitation or ion-exchange method. The structure of the as-synthesized samples and the presence of intended anions in the interlayer gallery of hydrotalcites were determined by X-ray diffraction and FTIR spectroscopy. On calcination at 600 °C the materials were transformed into mixed metal oxides. The kind of the counterbalancing anions present in the parent hydrotalcite influences strongly textural parameters of the obtained Mg-Al oxides. Both temperature-programmed desorption of NH₃ and CO₂, and test reaction of 2-methyl-3-butyn-2-ol (MBOH) conversion were used to determine the acidity and basicity of the samples. The hydrotalcite derived mixed Mg-Al oxides showed the presence of Brønsted and Lewis acid and base sites. However, the strong basic character of the solids caused that acetone and acetylene were observed as the major products of MBOH conversion.     

The reaction of ceria coatings on mica with H2S: An in-situ X-ray diffraction study

Thin layers of ceria were deposited on the surface of mica platelets in solution. The reaction of such particles with hydrogen sulfide yields a red colored special effect pigment. The ceria layer reacts with H₂S to produce a variety of sulfide and oxysulfide phases. The reaction path discovered in situ by time and temperature resolved X-ray diffraction is CeO₂→CeS₂→C-Ce₂S₃→Ce₁₀S₁₄O. The reaction itself is extremely variable depending on gas flow, heating rates and decomposition atmospheres. Effects on the thin film are recorded by scanning electron microscopy (SEM) and revealed a destruction of the layer once red Ce₁₀S₁₄O was formed. The product layer then reveals the typical nonwetting behaviour of a liquid on a surface.     

Synthesis of LiFePO4 with fine particle by co-precipitation method

LiFePO₄ is a potential candidate for the cathode material of the lithium secondary batteries. A co-precipitation method was adopted to prepare LiFePO₄ because it is simple and cheap. Nitrogen gas was needed to prevent oxidation of Fe²⁺ in the aqueous solution. The co-precipitated precursor shows the high reactivity with the reductive gas, and the single phase of LiFePO₄ is successfully synthesized with the aid of carbon under less reductive conditions. LiFePO₄ fine powder prepared by co-precipitation method shows high rate capability, impressive specific capacity and cycle property.     

Effects of gallia additions on sintering behavior of gadolinia-doped ceria

The effects of gallia additions on the sintering behavior of gadolinia-doped ceria were systematically investigated from the following aspects: the variation in sintered density, the variation in grain size, and the existing forms of Ga₂O₃ in CeO₂.Sintered density increased with increasing Ga₂O₃ content up to 5 mol.% and then it decreased with further addition of Ga₂O₃. Grain size also increased with increasing Ga₂O₃ content up to 5 mol.% and then decreased with further addition of Ga₂O₃. Decrease in grain size was caused by a pinning effect of Ga₂O₃ precipitation at grain boundaries. Lattice constant decreased with increasing Ga₂O₃ content up to 5 mol.%. This decrease will be due to the substitution of smaller Ga³⁺ ions for Ce⁴⁺ ions in the CeO₂ structure. According to the results obtained from scanning electron microscope (SEM) and X-ray diffraction (XRD) analyses, the solubility limit of Ga₂O₃ in Ce_0.8Gd_0.2O_1.9 ceramics can be estimated to be nearly 5 mol.%. The addition of Ga₂O₃ up to the solubility limit was found to promote the sintering properties of Gd₂O₃-doped CeO₂.     

Electrical conductivity and gas sensitivity of Zn-Sb-O thick films

The thick film of Zn-Sb-O was prepared by coating the paste of nanoparticles mixture (Sb₂O₃:ZnO=1:3) on the alumina substrate, followed by sintering at 500-900 °C for 2 h in air. The electrical resistance and gas-sensing properties to benzene, alcohol and acetone of Zn-Sb-O films were found to be dependent on the change of phase structure caused by sintering temperature.     

Assessing organo-clay dispersion in polymer layered silicate nanocomposites: A SAXS approach

A SAXS method for the quantitative assessment of the morphology of polymer layered silicate nanocomposites is proposed. Fitting the SAXS patterns, the number of clay layers, the periodicity of the layers in the tactoids, the thickness of the regions interposed between the clay platelets and their distributions can be measured. A good agreement with TEM data was obtained, avoiding the inconsistencies with microscopical observations often reported in the literature.     

Time dependent crystal-smectic transformation in perylene-containing polyimides

The crystalline conformations of perylene polyimides (PPIs), with alkyl spacers varying in length from C₃ to C₁₂ are discussed. Although modeling of single chains would suggest the possibility that those with odd number of CH₂ groups adopt a flat helical shape, X-ray diffraction suggests that the chains with odd and even spacers have the same conformation, due to the necessity to pack the perylene units. Upon annealing, the UV-vis absorption maximum red-shifts by about 10 nm, indicating enhanced π-stacking between the perylenes. Several changes in the spectra are seen with an increase in annealing time, at a given temperature. With an increase in annealing time, X-ray diffraction patterns show changes in the number of reflections, indicative of a crystal to mesogenic transition. The time required for this transition increases with a decrease in the spacer length, and annealing temperature, suggesting that the dynamics of this transition is very slow.