Study of the drying zirconia gel-precipitates using thermal analysis

Thermoanalytical techniques (TG, DTG, DTA and EGA) can be helpful in studying gel compositions and relating the chemical history and the role of the precipitant to the chemical properties of gels. The objective of our work was to determine the influence of the initial conditions in the reaction mixture on the product characteristics. Zirconia gels were prepared by the gelprecipitation method by the hydrolysis of zirconium tetrachloride dissolved in methanol. The substitution of water by methanol was chosen in order to obtain a reaction medium in which better control of the hydrolysis and condensation reactions of the zirconium precursor were achieved and thus also better control of the final properties of the dried zirconia gel-precipitates could be obtained. The nature of the hydrated zirconia gels obtained during the gelation process is strongly influenced by the conditions of the reaction mixture, e.g. concentration of the zirconium precursor, the mixing rate and particularly by the amount of water added. To distinguish between various types of water in the gel-precipitates, the furnace atmosphere and the partial water pressure were altered appropriately. It was shown that initial zirconium to water molar ratio has a significant effect on the properties of the final products. It was assumed that, according to the preparation conditions, three different types of water are present in the formed zirconia gel-precipitates. Modification of the dehydration processes of zirconia gel-precipitates enables control of the final microstructural and surface properties of the dried gels which are suitable for further catalysts support as well as mixed oxide preparation.     

Über Reaktionen von Nitrosophenolen, 3. Mitt.: Reaktion von 2-Nitroso-1-naphthol mit Resorcin und Orcin

Zusammenfassung Die Reaktion von 2-Nitroso-1-naphthol mit Resorcin bzw. Orcin in Äther bei Anwesenheit von HNO₃ liefert Benzo[c]phenoxazon-(9) (I), Benzo[c]phenoxazon-(9)-12-oxid (II), Methyl-benzo[c]phenoxazon-(9) (III) sowie 11-Methyl-benzo[c]phenoxazon-(9)-12-oxid (IV). Die Struktur der isolierten Substanzen wurde durch Reduktion mittels TiCl₃ sowie durch die UV- und IR-Spektren gestützt.

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The reaction of 2-nitroso-1-naphthol with resorcinol and orcinol in ether solution in the presence of nitric acid has been studied. From the reaction mixture the benzophenoxazones I–IV have been isolated. Structures were assigned on the grounds of UV and IR spectra and partly by using TiCl₃ as a reducing agent.

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Critical behaviour of the compressible magnet with exchange anisotropy

Then-component magnet with exchange anisotropy on a compressible lattice, with isotropic elastic properties, is studied. The renormalization group method is applied ind =4 — dimensions. The fixed points and the stability regions are explored to the order ², and the analysis is concentrated upon the casen<4—2 +O( ²). Investigation of the fixed points reveals various crossover phenomena which are not present in the corresponding rigid model. Renormalization of the anisotropy crossover exponent is demonstrated. It is shown that macroscopic instabilities, leading to the first order phase transition, may appear.     

Analytische Aspekte der Oxydation organischer Stickstoffverbindungen mit Chromsäure. II

Zusammenfassung Eine Halbmikromethode zur Bestimmung der an Kohlenstoff oder Sauerstoff gebundenen Nitro- und Nitrosogruppen in organischen Verbindungen wurde ausgearbeitet. Die Methode beruht auf dem oxydativen Aufschluß der Substanz mit einem Chromsäure—Schwefelsäure-Gemisch, wobei die Nitro- und Nitrosogruppen quantitativ in Salpetersäure übergehen. Diese wird mit Devarda-Legierung in alkalischem Medium zu Ammoniak reduziert, das dann im Stickstoffstrom abdestilliert und acidimetrisch titriert wird.

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Summary A semimicro method for determining nitro- and nitroso groups attached to carbon or oxygen in organic compounds has been worked out. The method is based on the oxidative decomposition of the sample with a chromic acid-sulfuric acid mixture, the nitro and the nitroso groups being quantitatively transformed into nitric acid. The latter is reduced to ammonia by means of Devarda alloy in alkaline medium, and is then distilled off in a stream of nitrogen and titrated with a standard acid solution.

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Résumé On a mis au point une méthode à l'échelle semimicro pour le dosage dans les substances organiques de groupes nitro et nitroso liés au carbone ou à l'oxygène. La méthode repose sur l'attaque oxydante de la substance par un mélange acide chromique-acide sulfurique, ce qui transforme quantitativement les groupes nitro et nitroso en acide nitrique. Au moyen de l'alliage de Devarda en milieu alcalin, on réduit celui-ci en ammoniac que l'on chasse par distillation dans un courant d'azote et que l'on titre par acidimétrie.

     

Mean value estimates in lattice point theory

LetQ(u) be a positive definite quadratic form inr2 variables with a real symmetric coefficient matrix of determinantD. Given a real vectorb with 0b _j <1, forx>0 letA(x) be the number of lattice points in the ellipsoidQ(u+b)x, letV(x) be the volume of this ellipsoid andP(x)=A(x)–V(x). Let . By introduction of a parameter we shall show how the treatment of estimates onP(x) and onM(x) can be unified.     

Magnetic moments and the high field susceptibilities of MnFe2O4

An extended version of the noncollinear spin model bySawatzky et al. is developed to derive a dependence of the differential high field susceptibility on the degree of inversion of the ferrite MnFe₂O₄. Using the available data on the main molecular field coefficients it is shown that the present model imposes restrictions on values of. Determination of from the measurements of the field dependence of the saturated moments at low temperatures on samples with varying degrees of inversion reveals good quantitative agreement with the present model.     

UV Light-induced Crosslinking of the Complementary Strands of Plasmid pUC19 DNA Restriction Fragments

Restriction fragments of pUC19 DNA were irradiated by various doses of UV light and analyzed by denaturing (alkaline) agarose gel electrophoresis. The irradiation generated retarded species whose mobility indicated two crosslinked DNA strands. Quantitative analysis of the experimental data provided an empirical equation relating the fraction of crosslinked DNA molecules to their length and to the dose of their irradiation by UV light. This equation can be used to predict the crosslinking behavior of pUC19-like DNA molecules whose primary structures do not much differ from a random nucleotide sequence. The amount of interstrand crosslinks increased with the (A+T) content of the pUC19 DNA fragments but the dependence was not clear-cut to indicate that oligonucleotide composition of DNA played a significant role as well.     

Extraction of Am(III) in the presence of lanthanides and yttrium by benzyldimethyldodecylammonium nitrate from acidic nitrate solutions

We have investigated the effect of coextraction of lanthanides and yttrium on the distribution coefficients D_Am in the extraction of americium by benzyldimethyldodecylammonium nitrate (BDMLNNO₃) from nitrate solutions. In the coextraction of lanthanides, the extraction of Am(NO₃)₃ is suppressed, which is markedly manifested in the extraction of light lanthanides (La, Ce, Pr); of the series of lanthanides their extraction is the highest. The effect of nitric acid and the possibility of separation of lanthanides and americium by the application of three-stage multiple extraction is discussed.     

Distribution of fallout radionuclides through soil surface layer

The distribution of¹³⁷Cs through soil layers has been investigated by field sampling. The investigation deals with¹³⁷Cs concentration found after the Chernobyl accident. The relationship between important soil characteristics, total precipitation and cesium distribution are analyzed. Cesium is strongly sorbed in the top soil layer and its migration downward is limited. Measurements performed over a 3-year period revealed that approximately 20–38 per cent of total¹³⁷Cs is located in the upper soil layer.