Untersuchungen über Perylen und seine Derivate

Ohne Zusammenfassung     

tert‐Butyl (6S)‐4‐hydroxy‐6‐isobutyl‐2‐oxo‐1,2,5,6‐tetra­hydropyridine‐1‐carboxyl­ate and tert‐butyl (4R,6S)‐4‐hydroxy‐6‐iso­butyl‐2‐oxopiperidine‐1‐carboxyl­ate

X‐ray studies reveal that tert‐butyl (6S)‐6‐iso­butyl‐2,4‐dioxo­piperidine‐1‐carboxyl­ate occurs in the 4‐enol form, viz. tert‐butyl (6S)‐4‐hydroxy‐6‐iso­butyl‐2‐oxo‐1,2,5,6‐tetra­hydropyri­dine‐1‐carboxyl­ate, C₁₄H₂₃NO₄, when crystals are grown from a mixture of di­chloro­methane and pentane, and has an axial orientation of the iso­butyl side chain at the 6‐position of the piperidine ring. Reduction of the keto functionality leads predominantly to the corresponding β‐hydroxy­lated δ‐lactam, tert‐butyl (4R,6S)‐4‐hydroxy‐6‐iso­butyl‐2‐oxo­piperidine‐1‐car­boxyl­ate, C₁₄H₂₅NO₄, with a cis configuration of the 4‐hydroxy and 6‐iso­butyl groups. The two compounds show similar molecular packing driven by strong O—H⋯O=C hydrogen bonds, leading to infinite chains in the crystal structure.     

Determination of temperature by stimulated raman scattering of molecular nitrogen,oxygen, and carbon dioxide

We have determined the temperature from SRS spectra of N₂-N₂, N₂-CO₂, O₂-O₂, and CO₂-CO₂ recorded in wide pressure and temperature ranges. The fitting procedure takes simultaneously into account the Dicke effect and motional narrowing. We have quantified the accuracy of the MEG and ECS-P models for rotational relaxation. The temperature extracted from each model is compared with thermocouple measurements. The influence of vibrational broadening and shifting is discussed in detail.     

Oxygen inhibition in thiol–acrylate photopolymerizations

The overall effects of oxygen on thiol–acrylate photopolymerizations were characterized. Specially, the choice of thiol monomer chemistry, functionality, and concentration on the extent of oxygen inhibition were considered. As thiol concentration was increased, the degree of oxygen inhibition was greatly reduced because of chain transfer from the peroxy radical to the thiol. When comparing the copolymerization of 1,6‐hexanediol diacrylate with the alkane‐based thiol (1,6‐hexane dithiol) to the copolymerization with the propionate thiol (glycol dimercaptopropionate), it was found that the propionate system was much more reactive and polymerized to a greater extent in the presence of oxygen. In addition, the functionality was considered where the glycol dimercaptopropionate was compared to a tetrafunctional propionate of similar chemistry (pentaerythritol tetrakis(mercaptopropionate)). Given the same thiol concentration, the higher functionality thiol imparted a faster polymerization rate, due to the increased polymer system viscosity, which limited oxygen diffusion and decreased the extent of overall oxygen inhibition. Thus, preliminary insight is provided into how thiol monomer choice affects the extent of oxygen inhibition in thiol–acrylate photopolymerization. © 2006 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 44: 2007–2014, 2006     

Separation and analysis of radioiodine in nuclear reprocessing solutions of high ionic strength

Ion chromatography (IC) can be used to separate radioiodine from fission products and other ionic species in complex reprocessing solution matrices. A preliminary concentration and separation of the radioiodine is performed using a column filled with a platinum-coated copper bed which converts all forms of iodine to iodide and selectively adsorbs the iodide. The separation is completed by employing an anion chromatographic system. The iodide peak aliquot is collected for subsequent radioanalysis by low energy photon spectroscopy. Results indicate quantitative separation and recovery of iodine. The entire system is automated under computer control and is able to handle small (l) and large (500 ml) sample sizes.     

La méthyl-9-trihydroxy-2,3,7-fluorone-6, réactif microqualitatif de l'antimoine

Résumé La méthyl-9-trihydroxy-2,3,7-fluorone-6 permet de déceler les ions de l'antimoine, en présence de tous autres cations et anions. Les conditions deph (ph = 4) sont à observer rigoureusement.Ce nouveau réactif est avantageusement utilisé dans la méthode d'analyse à la touche ou par empreinte.Les limites de sensibilité sont: en godet 0,2; sur papier gélatine 0,5; sur papier filtre 0,8.

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Summary Methyl-9-trihydroxy-2,3,7-fluorone-6 is a reagent which allows to detect antimony ion in the presence of all the other cations and anions. Aph value of 4 must be strictly maintained.This new reagent can be advantageously applied for spot test and offprint analysis.Limits of identification: On the spot test plate 0,2; On gelatine paper 0,5; On filter paper 0,8.

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Zusammenfassung Das Methyl-9-trioxy-2,3,7-fluoron-6 gestattet den Nachweis des Antimonions in Gegenwart aller anderen Kationen und Anionen. Dieph-Bedingungen (ph = 4) sind streng einzuhalten.Dieses neue Reagens läßt sich mit Vorteil zur Tüpfel- oder Abdruckanalyse verwenden.Erfassungsgrenzen: auf der Tüpfelplatte 0,2; auf Gelatinepapier 0,5; auf Filtrierpapier 0,8.