Chemische Zusammensetzung und Mikrostruktur polymerabgeleiteter Gläser und Keramiken im System Si–C–O. Teil 2: Charakterisierung der Gefügeausbildung mittels hochauflösender Durchstrahlungselektronenmikroskopie und Feinbereichsbeugung

Chemical Composition and Microstructure of Polymer‐Derived Glasses and Ceramics in the Si–C–O System. Part 2: Characterization of microstructure formation by means of high‐resolution transmission electron microscopy and selected area diffraction Liquid or solid silicone resins represent the economically most interesting class of organic precursors for the pyrolytic production of glass and ceramics materials on silicon basis. As dense, dimensionally stable components can be cost‐effectively achieved by admixing reactive filler powders, chemical composition and microstructure development of the polymer‐derived residues must be exactly known during thermal decomposition. Thus, in the present work, glasses and ceramics produced by pyrolysis of the model precursor polymethylsiloxane at temperatures from 525 to 1550 °C are investigated. In part 1, by means of analytical electron microscopy, the bonding state of silicon was determined on a nanometre scale and the phase separation of the metastable Si–C–O matrix into SiO₂, C and SiC was proved. The in‐situ crystallization could be considerably accelerated by adding fine‐grained powder of inert fillers, such as Al₂O₃ or SiC, which permits effective process control. In part 2, the microstructure is characterized by high‐resolution transmission electron microscopy and selected area diffraction. Turbostratic carbon and cubic β‐SiC precipitate as crystallization products. Theses phases are embedded in an amorphous matrix. Inert fillers reduce the crystallization temperature by several hundred °C. In this case, the polymer‐derived Si–C–O material acts as a binding agent between the powder particles. Reaction layer formation does not occur. On the investigated pyrolysis conditions, no crystallization of SiO₂ was observed.     

Microstructure of Feta Cheese Made Using Different Cultures as Determined by Confocal Scanning Laser Microscopy

ABSTRACT: The objective of this work was to observe the microstructure of feta cheese using confocal scanning laser microscopy. Low fat cheese and cheese containing capsule-producing cultures were made. The protein network was observed using the reflectance mode of the confocal microscope. Fat was stained by Nile red dye diluted with whey. More even distribution of fat with a larger number of smaller globules was observed in cheese made with noncapsule-forming culture compared to that made with the capsule-forming culture. Nonfat cheese had compact structure when made with noncapsule-forming culture which contrasted with the open structure observed in cheese made with the capsule-forming culture     

Biodegradation of monoaromatic hydrocarbons in aquifer columns amended with hydrogen peroxide and nitrate

The ability of indigenous microorganisms to degrade benzene, toluene, ethylbenzene and xylenes (BTEX) in laboratory scale flow-through aquifer columns was tested separately with hydrogen peroxide (110 mg/l) and nitrate (330 mg/l as NO₃⁻) amendments to air-saturated influent nutrient solution. The continuous removal of individual components from all columns relative to the sterile controls provided evidence for biodegradation. In the presence of hydrogen peroxide, the indigeneous microorganisms degraded benzene and toluene (> 95%), meta- plus para-xylene (80%) and ortho-xylene (70%). Nitrate addition resulted in 90% removal of toluene and 25% removal of ortho-xylene. However, benzene, ethylbenzene, meta- and para-xylene concentrations were not significantly reduced after 42 days of operation. Following this experiment, low dissolved oxygen (< 1 mg/l) conditions were initiated with the nitrate-amended column influent in order to mimic contaminated groundwater conditions distal from a nutrient injection well. Toluene continued to be effectively degraded (> 90%), and more than 25% of the benzene, 40% of the ethylbenzene, 50% of the meta- plus para-xylenes and 60% of the ortho-xylene were removed after several months of operation.     

Intracellular localization of the antitumour drug adriamycin in living cultured cells: A confocal microscopy study

The intracellular distribution of the anthracyclinic antibiotic adriamycin in living cultured cells has been investigated by confocal microscopy. In human melanoma cells (M14), adriamycin was localized inside the nuclei. When adriamycin-treated M14 cells were allowed to recover in drug-free medium, a complete efflux of the drug from the nucleus was revealed. In recovered cells, a weakly fluorescent signal was observed in the perinuclear region. When M14 cells were recovered in a medium containing colcemid, a microtubule depolymerizing agent, the drug transport from the nucleus to the cell periphery appeared to be inhibited, suggesting that the microtubule network is strongly involved in drug transport mechanisms. In multidrug-resistant (MDR) cells the intracellular location of adriamycin was shown to be noticeably different from that of the parental wild-type cells. In particular, in resistant human breast carcinoma cells (MCF-7), adriamycin appeared to be exclusively located within the cytoplasm whereas the nuclei were shown to be completely negative. When adriamycin treatment was performed in association with MDR revertants, such as Lonidamine (inhibitor of the energy metabolism) or verapamil (inhibitor of the P-glycoprotein efflux pump), a marked enhancement of the cytoplasmic signal was observed in resistant cells. Under these conditions, adriamycin appeared concentrated in the perinuclear region, but the nuclei were still negative. Confocal microscopy proved to be a very useful method for the study of the intracellular transport of fluorescent substances, such as anthracyclinic antibiotics, and for the investigation of the multidrug resistance phenomenon in tumour cells.     

High temperature controlled atmosphere experiments for catalysts in a transmission electron microscope

A new transmission electron microscopy (TEM) specimen preparation procedure for high temperature experiments using a controlled atmosphere specimen holder (HTCASH) has been developed. It is designed for studying the microstructure of catalyst specimens before and after treatments in various gases. The procedure involved (1) finding a new formula for the embedding material, (2) devising a new method of making specimen supports, and (3) developing a method for removing the embedding material after the specimen has been microtomed. These techniques were then brought together to produce the ideal specimens for the HTCASH experiments. As an extra benefit, this procedure is also suitable for preparing specimens for ultrahigh resolution imaging experiments. The application of the new procedure in HTCASH experiments is illustrated through a high temperature reduction of a Co/SiO₂-923 catalyst.     

Intercomparison of scanning probe microscopes

Comparison measurements on reference standards are reported in which 13 partners with different instruments took part. A set of prototype standards which had been produced and calibrated within a European project were used for the measurements. Here, results of measurements on a 240 nm step height standard and a two-dimensional lateral standard with a nominal pitch of 1 μm are reported.     

摩擦强度对薄膜表面形态的作用:原子力显微镜下的观察

展示了摩擦强度对聚酰亚胺薄膜表面形态的影响，原子力显微图像显示，机械摩擦会使聚酰亚胺薄膜表面上形成微沟槽，这些沟槽的表面具有丰富的表面精细构造。原子显微图像还揭示了机械摩擦可以改变被磨擦聚酰亚胺膜的表面形态。     

Influence of Edible Films upon the Moisture Loss and Microstructure of Dietetic Sucrose-Free Sponge Cakes during Storage

The kinetics of changes in the bound water content in dietetic sucrose-free sponge cakes (DC) during storage was investigated. The effect of edible films of polymyxan, pectin, xanthan, and carboxymethylcellulose upon this kinetics was also investigated. The quantitative changes in both states of water (slightly bound water and strongly bound water) were registered by combined dynamic analysis (thermogravimetry analysis, TGA, and differential thermal analysis, DTA). The moisture changes in DC crumb were analyzed by drying out to constant mass. The rate constants were determined according the equation q = q_oe^-kt. The values of rate constants 'k', in day^-1, concerning the different edible films were as follows: for crumb moisture is (8.00 ≤ k ≤ 12.47) × 10^-3, for bound water is (3.07 ≤ k_w ≤ 6.26) × 10^-2, for slightly bound water is (4.22 ≤ k₁ ≤ 8.49) × 10^-2 and for strongly bound water is (2.02 ≤ k₂ ≤ 5.62) × 10^-2 as compared to 18.53 × 10^-3, 7.16 × 10^-2, 9.04 × 10^-2, and 5.36 × 10^-2 in the uncovered DC, respectively. The best water-retaining effect in respect to crumb moisture during storage was ascertained in the use of polymyxan and xanthan films. The lowest rate constant values for bound water and its two states were measured for DC covered with pectin. The relation between the kinetics of both bound water states during storage and ageing of the crumb of DC covered with different edible films and the crumb microstructure was represented. By means of scanning electron microscope was read the smallest change in crumb microstructure of pectin-covered DC on the sixth day of storage.     

Influence of accelerated ageing on methacrylate‐based denture resins heterogeneity as viewed by ESR‐spin‐probe method

The electron‐spin‐resonance (ESR) spin‐probe method, was used to study the heterogeneity of denture resins based on poly(methyl methacrylate). Results for three resins processed by microwave energy, conventional curing and cold curing (depending on the curing procedure and exposed to ageing in various environmental conditions) were compared. All three cured resins were stored over the same time (1200 h) in distilled water at ambient temperature and in artificial saliva at 348 K. The temperature‐dependent ESR spectra of a spin probe dispersed in the denture resins are analyzed in terms of line‐shapes and line‐widths. The appearance of two spectral components was taken as an indication of resin heterogeneity. The results reveal that the cold‐cured resin has a lower local density in comparison with microwave and conventionally cured resin. The amount of residual monomer also contributes to the local motion of polymer segments. The change of denture resins exposed to ageing is influenced both by the structure of the original resin and the ageing conditions. Restricted motion of a spin probe incorporated into the acrylic resins exposed to accelerated ageing suggests additional crosslinking of polymer chains. The differences are observed for all the investigated resins, but the highest change is observed with the cold‐cured resin. The ESR results are accompanied by T_g and T_m measurements. Copyright © 2005 Society of Chemical Industry     

A simple handling technique for mammalian oocytes and embryos during preparation for transmission electron microscopy

Due to their small size, mammalian oocytes and embryos pose unique problems during preparation for transmission electron microscopy. This paper outlines a method which combines protein embedding with centrifugation to locate the specimens on the face of a Beem capsule mould. This method facilitates both the processing of oocytes with minimal loss and rapid location of the specimens within the block for simultaneous sectioning, staining and examination.