Infrared and ultraviolet–visible spectroscopic studies of silica, [(Cp)2ZrCl2] and trimethylaluminum interactions

Infrared and UV–vis studies of metallocene immobilization on silica are reported here. The results have indicated changes in the Zr coordination sphere of metallocene depending on the immobilization route used. The reaction of [(Cp)₂ZrCl₂] with silica formed [(Cp)₂ZrCl]⁺[SiO]⁻ species. The same metallocene, reacting with TMA modified silica, formed monomethylated and dimethylated species by the substitution of chloro for methyl ligands, stabilized on the surface by interaction with “MAO-like” species (methylaluminoxane, MAO). These monomethylated and dimethylated cationic zirconium species are the active centers for the polymerization reaction. Different order of TMA addition in the silica modification step generated surface species of a similar nature, differing in their relative quantities. The highest amount of these active species was obtained when the support was added to the TMA solution rather than adding the TMA solution to the silica support. This was the most significant parameter affecting catalytic activity in ethylene polymerization.     

刚性棒状全芳香液晶聚酯的合成及性质的研究

以溴和苯基取代的对苯二甲酰氯及2，2′-二甲基联苯-4，4′-二甲酰氯作为单体，分别与甲基、叔丁基、苯基取代的对苯二酚经熔融缩聚反应，合成一类具有刚性棒状结构的全芳香液晶聚酯。聚酯的热性质以TGA、DSC，热台偏光显微镜研究。所有的聚酯均为热致性液晶，它们具有相对较低的转变温度，在普通的有机溶剂中具有较好的溶解性质。     

Kinetic studies on strawberry anthocyanin hydrolysis by a thermostable anthocyanin-β-glycosidase from Aspergillus niger

Several kinetic characteristics of a thermostable anthocyanin-β-glycosidase from Aspergillus niger have been evaluated. With strawberry anthocyanins as substrate, at pH optimum (4·0) and t = 30°C, K_m was found to be $\text{123 ± 4 μ}\text{m}$ and V_max, 1·16 ± 0·06 μmol min^?1mg^?1 protein. Temperature optimum was observed at about 68°C. The apparent energy of activation was calculated to be 11 ± 1 kcal/mol. The inhibitory effect of different sugars and sugar derivatives was examined. Glucono-deltalactone ($\text{K}{}_{\mathrm{<mtext>i</mtext>}}\text{= 2·3 ± 0·1 μ}\text{m}$), gluconic acid ($\text{K}{}_{\mathrm{<mtext>i</mtext>}}\text{= 82 ± 2 μ}\text{m}$) and glucose ($\text{K}{}_{\mathrm{<mtext>i</mtext>}}\text{= 1·3 ± 0·1}\text{m}\text{m}$) appeared to be competitive inhibitors of this enzyme.     

Entschwefelung von gerührtem und ungerührtem Roheisen mit kalkreicher Schlacke unter oxidierender Gasatmosphäre

Aus Betriebsergebnissen bei der Pfannenentschwefelung ist ein negativer Einfluß oxidierender Gasphasen bekannt. Daher war es das Ziel der eigenen Untersuchungen in einer geeigneten Apparatur die Wirkung oxidierender Bedingungen in der Gasphase sowohl auf den Verlauf des Schwefelabbaues in der Schlacke als auch des Schwefeltransportes aus dem Roheisen in die Schlacke zu untersuchen. Oxidierende Gasphasen erwirken bei der Pfannenentschwefelung an der Phasengrenze Schlacke/Gas eine Oxidation des Schwefels aus der Schlacke, ohne jedoch bei ruhender Schlackenschicht ein Oxidationspotential in der Schlacke aufzubauen, das bis zur Phasengrenze Roheisen/Schlacke durchgreift und dort die Entschwefelung des Roheisens durch die Siliciumgehalte stört. Sowohl die Entschwefelung des Roheisens als auch die Oxidation des Schwefels aus der Schlacke werden durch höhere Temperaturen und durch eine Rührwirkung gefördert. Der Schwefeltransport wird bei den ungerührten wie bei den gerührten Schmelzen durch Diffusionsvorgänge gesteuert und auch hier durch steigende Temperaturen und rührende Kräfte begünstigt.     

Imaging the domain pattern of the canted magnetization state in Co/Pt multilayer films

The exact magnetization pattern of magnetic films close to a spin-reorientation transition is difficult to analyze due to the intrinsically three-dimensional (3d) variation of the orientation of the local magnetization. We present a technique how this can be performed, based on the analysis of high quality 2d polarization maps from a single scanning electron microscope with polarization analysis (SEMPA) measurement with tilted sample. The key tool is the statistical distribution of all occurring polarization doublets, visualized in a 2d histogram plot. From the shape of the distribution the type of transition—canted-phase, or coexisting phases—can be inferred. For the canted-phase state, the canting angle can be accurately determined from geometrical considerations. With help of the histogram the image data can be analyzed and the three components of the magnetization can be calculated for most points of the image. For a Co/Pt multilayer film we found a cone state. The magnetization forms a complex pattern consisting of out-of-plane domains while the in-plane magnetization shows a maze pattern.     

Interlaboratory ring test of time-resolved fluoroimmunoassays for zeranol and alpha-zearalenol and comparison with zeranol test kits.

Many zeranol immunoassay test kits cross-react with toxins formed by naturally occurring Fusarium spp. fungi, leading to false-positive screening results. This paper describes the evaluation and application of recently published, dry reagent time-resolved fluoroimmunoassays (TR-FIA) for zeranol and the toxin alpha-zearalenol. A ring test of bovine urine fortified with zeranol and/or alpha-zearalenol in four European Union National Reference Laboratories demonstrated that the TR-FIA tests were accurate and robust. The alpha-zearalenol TR-FIA satisfactorily quantified alpha-zearalenol in urine fortified at 10-30 ng ml(-1). The specificity-enhanced zeranol TR-FIA accurately quantified zeranol in the range 2-5 ng ml(-1) and gave no false-positive results in blank urine, even in the presence of 30 ng ml(-1) alpha-zearalenol. Zeranol TR-FIA specificity was demonstrated further by analysing incurred zeranol-free urine samples containing natural Fusarium spp. toxins. The TR-FIA yielded no false-positive results in the presence of up to 22 ng ml(-1) toxins. The performance of four commercially available zeranol immunoassay test kits was more variable. Three kits produced many false-positive results. One kit produced only one potential false-positive using a protocol that was longer than that of the TR-FIA. These TR-FIAs will be valuable tools to develop inspection criteria to distinguish illegal zeranol abuse from contamination arising from in vivo metabolism of Fusarium spp. toxins.