Glass forming region in the GeSe2–GeTe–PbTe system and some physicochemical properties of glassy alloys

New chalcogenide glasses from the GeSe₂–GeTe–PbTe system were synthesized. The glass forming region was determined using visual, X-ray diffraction and scanning electron microscopy analyses. It is extended towards the GeSe₂ and lies partially on the GeSe₂–GeTe (0–58 mol% GeTe) and GeSe₂–PbTe (20.0–57.5 mol% PbTe) sides. No glasses were obtained in the GeTe–PbTe system. The investigated physicochemical properties vary between 4.04–6.21 g/cm³ (density, d); 97–121 kgf/mm² (microhardness, HV); ?0.187 ÷ 0.007 (compactness, C) and 14.3–17.8 GPa (elasticity modulus, E), respectively.     

On smooth foliations with Morse singularities

Let M be a smooth manifold and let F be a codimension one, C^∞ foliation on M, with isolated singularities of Morse type. The study and classification of pairs (M,F) is a challenging (and difficult) problem. In this setting, a classical result due to Reeb (1946) [11] states that a manifold admitting a foliation with exactly two center-type singularities is a sphere. In particular this is true if the foliation is given by a function. Along these lines a result due to Eells and Kuiper (1962) [4] classifies manifolds having a real-valued function admitting exactly three non-degenerate singular points. In the present paper, we prove a generalization of the above mentioned results. To do this, we first describe the possible arrangements of pairs of singularities and the corresponding codimension one invariant sets, and then we give an elimination procedure for suitable center-saddle and some saddle-saddle configurations (of consecutive indices).In the second part, we investigate if other classical results, such as Haefliger and Novikov (Compact Leaf) theorems, proved for regular foliations, still hold true in presence of singularities. At this purpose, in the singular set, Sing(F) of the foliation F, we consider weakly stable components, that we define as those components admitting a neighborhood where all leaves are compact. If Sing(F) admits only weakly stable components, given by smoothly embedded curves diffeomorphic to S¹, we are able to extend Haefliger?s theorem. Finally, the existence of a closed curve, transverse to the foliation, leads us to state a Novikov-type result.     

Correlation Between Autofluorescence Intensity and Tumor Area in Mice Bearing Renal Cell Carcinoma

Protoporphyrin IX (PpIX) is a porphyrin derivative that is accumulated in cancerous tissue in consequence of the tumor-specific metabolic alterations. The aim of this study was to evaluate the accumulation of PpIX in mice bearing renal cell carcinoma by spectroscopy analysis. A total of 24 male Balb/c mice, 6 weeks old, were divided into six groups: Normal (without inoculation of tumor cells) and 4, 8, 13, 16, and 20 days after inoculation of tumor cells. The orthotopic tumor model of renal cancer was used. Murine renal cell carcinoma (Renca cells) were inoculated into the subcapsular space of the kidney. Normal and tumor-bearing kidneys in different progression stages were removed and analyzed by ex-vivo spectroscopy and by microscopy, for tumor histometric analysis. Emission spectra were obtained by exciting the samples at 405 nm. Significant differences between normal and tumor-bearing kidneys in autofluorescence shape occurred in the 600–700 nm spectral region. A good correlation was found between emission band intensity at 635 nm and the tumor area.     

Determination of pyrimethanil and kresoxim-methyl in green groceries by headspace solid-phase microextraction and gas chromatography-mass spectrometry

A method for determination of trace amounts of the fungicides pyrimethanil and kresoxim-methyl in green groceries, previous headspace solid-phase microextraction (HSSPME), was developed using gas chromatography-mass spectrometry and selected ion monitoring (GC-MS, SIM). Both fungicides were extracted with a fused-silica fiber coated with 85 microm polyacrylate. The effects of pH, ionic strength, extraction and desorption times as well as the extraction temperature were studied. The linear concentration range of application was 12.5-250 ng g(-1) for both compounds, with detection limits of 1.8-2.0 ng g(-1) for pyrimethanil and 2.8-3.1 ng g(-1) for kresoxim-methyl. SPME/GC-MS analysis yielded good reproducibility (RSD between 7.4 and 15.0%). It was applied to check the eventual existence of pyrimethanil and kresoxim-methyl above the detection limits on grapes, strawberries, tomatoes and ketchup samples. The method validation was completed with spiked matrix samples. It can be applied as a monitoring tool in grapes, strawberries, tomatoes and ketchup samples.     

Global Solar UV Index: Australian measurements, forecasts and comparison with the UK

The 2002 revision of the UV index (UVI) issued by the World Health Organisation (WHO), the World Meteorological Office (WMO), the United Nations Environment Programme (UNEP) and the International Commission on Non-Ionizing Radiation Protection (ICNIRP) (World Health Organization [2002] Global Solar UV Index: A Practical Guide. WHO, Geneva) was motivated by the need to further standardize the use and presentation of the UVI. Awareness of the hazards of solar UV radiation (UVR) is generally high in Australia, but more effective use of the UVI will assist in promoting further changes to the population's sun exposure behavior. UVI levels for a number of cities around Australia as measured by the Australian Radiation Protection and Nuclear Safety Agency (ARPANSA), covering the time period 1996-2000, are presented. Also shown are UVI forecasts from the Australian Bureau of Meteorology (BOM). Agreement between the BOM data and the measurements varies depending on the location but is within 2 UVI units approximately 75% of the time. UVI levels are supplied to the media, and in summer values in excess of 12-14 are regularly recorded, although the more northerly locations occasionally reach 16 and 17. The factors affecting the solar UVR environment and the measured UVI are also discussed and compared against measurements from the UK.     

Michael reaction. V. Stereochemistry of the NaNH2 catalyzed two-step reaction between phenylacetic acid dialkyl amides and methyl cinnamate or cinnamic acid dialkyl amides

The reaction is investigated between sodium-metallated (NaNH₂) phenylacetic acid dialkyl amides and methyl cinnamate or cinnamic acid dialkyl amides. The thermodynamic equilibrium between the diastereomeric 2,3-diphenylglutaric acid amidoesters or diamides is 5/95 in favour of thethreo-isomer. Under kinetic conditions the stereochemistry of the reaction depends on the nature of the donor and the solvent.

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Michael Reaktion. V. Stereochemie der durch NaNH₂ katalysierten zweistufigen Reaktion zwischen Dialkylamiden der Phenylessigsäure und Methylestern oder Dialkylamiden der Zimtsäure

Zusammenfassung Die Umsetzung zwischen der mit festem NaNH₂ gewonnenen Natriumderivaten der Dialkylamiden der Phenylessigsäure und Methylestern oder Dialkylamiden der Zimtsäure wurde untersucht. Das thermodynamischeE/T-Verhältnis zwischen den gewonnenen diastereomeren Amidestern und Diamiden der 2,3-Diphenylglutarsäure beträgt in allen Fällen 5/95. Das stereochemische Ergebnis unter kinetischen Bedingungen hängt von der Natur des Donators und von den Lösungsmitteln ab.

     

Determination of germanium after extraction by Methyl Isobutyl Ketone. I

Summary The extractability of germanium from 7.5 N hydrochloric acid solutions by methyl isobutyl ketone has been studied and applied to the separation of small amounts of this element. The extracted germanium tetrachloride reacts with ammonium molybdate. The germanomolybdic acid formed dissolves in the organic phase where it is directly reduced with ascorbic acid. Very stable blue solutions are obtained. A number of interfering ions are separated by preliminary extraction of the cupferrates with the same solvent. Phosphate ions are removed by previous precipitation with zirconyl nitrate. Arsenate is reduced to arsenite and indirect interference of fluoride is avoided by addition of aluminum chloride. The extraction technique employed is very simple and the method is applicable to the determination of germanium in flue dusts and other complex silicon materials without previous separation of silicon.

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Zusammenfassung Die Extrahierbarkeit von Germanium aus 7,5-n Salzsäure mit Methylisobutylketon wurde untersucht und auf die Abtrennung kleiner Mengen dieses Elementes angewendet. Das extrahierte Germaniumtetrachlorid reagiert mit Ammoniummolybdat. Die entstehende Germaniummolybdänsäure löst sich in der organischen Phase und wird dort unmittelbar mit Ascorbinsäure reduziert. Man erhält hierbei sehr stabile blaue Lösungen. Eine Reihe störender Ionen wird durch vorhergehende Extraktion der Cupferronate mit dem gleichen Lösungsmittel entfernt. Phosphationen werden vorher mit Zirkonylnitrat ausgefällt. Arsenat wird zu Arsenit reduziert. Indirekte Störung durch Fluorid vermeidet man durch Zugabe von Aluminiumchlorid. Das angegebene Extraktionsverfahren ist sehr einfach und die Methode zur Bestimmung von Germanium in Flugstaub und anderen komplexen Siliciummaterialien ohne vorherige Abtrennung des Siliciums verwendbar.

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Résumé Etude de la possibilité d'extraction du germanium de solutions chlorhydriques acides 7,5 N par la méthylisobutylcétone et application à la séparation de petites quantités de cet élément. Le tétrachlorure de germanium ainsi extrait réagit sur le molybdate d'ammonium. L'acide germanomolybdique formé se dissout dans la phase organique dans laquelle il est directement réduit par l'acide ascorbique. On obtient des solutions bleues très stables. Un certain nombre d'ions gênants sont séparés par une extraction préalable de cupferronates dans le même solvant. Les ions phosphoriques sont éliminés par précipitation préalable par le nitrate de zirconyle. Les arséniates sont réduits en arsénites. La perturbation indirecte des fluorures est évitée par addition de chlorure d'aluminium. La technique d'extraction utilisée est très simple et la méthode est applicable à la détermination du germanium dans les poussières de foyers ou autres substances siliciées complexes sans séparation préalable du silicium.

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Presented in part at the national meeting of the Sociedade Brasileira para o Progresso da Ciência held in Curitiba, Brazil, November 1953.     

Validation of a headspace trap gas chromatography and mass spectrometry method for the quantitative analysis of volatile compounds from degraded rapeseed oil

Due to lipid oxidation, off‐flavors, characterized by a fishy odor, are emitted during the heating of rapeseed oil in a fryer and affect the flavor of rapeseed oil even at low concentrations. Thus, there is a need for analytical methods to identify and quantify these products. To study the headspace composition of degraded rapeseed oil, and more specifically the compounds responsible for the fishy odor, a headspace trap gas chromatography with mass spectrometry method was developed and validated. Six volatile compounds formed during the degradation of rapeseed oil were quantified: 1‐penten‐3‐one, (Z)‐4‐heptenal, hexanal, nonanal, (E,E)‐heptadienal, and (E)‐2‐heptenal. Validation using accuracy profiles allowed us to determine the valid ranges of concentrations for each compound, with acceptance limits of 40% and tolerance limits of 80%. This method was then successfully applied to real samples of degraded oils.     

Synthesis and electric properties of the high-k ceramic composites based on potassium polytitanate modified by manganese

Research on Chemical Intermediates - Potassium polytitanates powders were modified by treatment in aqueous solutions of manganese sulfate at different pH, the obtained intermediates (PPT/Mn) were...