The use of liquid scintillation spectrometry for the determination of radionuclidic purity of 90Y from a radiochemical 90Y/90Srgenerator

Summary An extraction technique for the separation of ⁹⁰Sr from a high excess of⁹⁰Y has been developed. This procedure can be used for the determination of trace amounts of⁹⁰Sr in⁹⁰Y prepared by a radiochemical⁹⁰Y/⁹⁰Sr generator by liquid scintillation.     

Extraction separation of strontium and yttrium radionuclides by hydrogen heptachlorodicarbollylcobaltate in the presence of benzo-15-crown-5

Extraction of strontium and yttrium by the nitrobenzene solution of H⁺-form of heptachloro-bis-1,2-dicarbollylcobaltate (H⁺B^–) in the presence of benzo-15-crown-5 (B15C5, L) has been investigated. The presence of B15C5 leads to a great synergistic effect for the extraction of strontium and an antagonistic effect for the extraction of yttrium. The extraction constants of Sr²⁺ complexes of B15C5 were determined. The separation factor a(Sr/Y) in the system with B15C5 presents the same order of magnitude as that for 15C5.     

The infrared spectra and normal coordinate analysis of syn and anti acetaldoxime

The infrared spectra of mixtures of syn and anti acetaldoxime and its deuterated analogues CH₃CHNOD, CD₃CHNOH, CD₃CDNOH and CH₃CDNOH have been recorded. The syn and anti isomers of CH₃CHNOH, CD₃CHNOH, CD₃CDNOH and CH₃CDNOH have been separated by gas chromatography [1]. The infrared spectra of separated isomers in CS₂ solution have been recorded and the assignment of ten in-plane vibrations made. From a normal coordinate analysis the Urey-Bradley force field, the potential energy distribution and additional information about assignments have been obtained.For the anti isomer the simple Urey-Bradley force field gives satisfactory agreement between the calculated and measured frequencies. For the syn isomer it is necessary to take into account the interactions between atoms separated by three bonds.     

Ein weiterer Beitrag zum Scandiumdicarbidproblem

Zusammenfassung Die bei 1850, 2000 bzw. 2300°C durch die Reduktion von Scandiumoxid mittels Kohlenstoff in dem der Scandiumdicarbidbildung entsprechenden Molverhältnis hergestellten Produkte wurden mit Wasser zersetzt und mit Hilfe der gleichzeitigen gaschromatographischen und massenspektrometrischen Analyse untersucht. Aus den Ergebnissen geht hervor, daß bei der Scandiumdicarbidbildung gleichzeitig ein weiteres Scandiumcarbid, höchstwahrscheinlich ein Sesquicarbid, entsteht.

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Scandium(III) dicarbide problem. Further experimental results

Products obtained by the reduction of Sc₂O₃ with carbon at 1850, 2000 and 2300°C, resp., in the molar ratio corresponding to the scandium dicarbide were hydrolysed with water. Gaseous reaction products were analysed using gas chromatography combined with mass spectrometry. Results show, that during dicarbide formation another scandium carbide, probably sesquicarbide, is also formed.

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Herrn Prof. Dr.H. Nowotny gewidmet.

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7. Mitt.: Coll. Czech. Chem. Commun., im Druck.     

Über komplexe Fällungserscheinungen der Silberphosphat-Sole in statu nascendi

Zusammenfassung Es wurden Fällungssysteme Silbernitrat-Alkaliphosphat und Silbernitrat-Alkaliphosphat-Kaliumbromid tyndallometrisch untersucht, wobei festgestellt wurde, daß sich in dem Fällungssystem AgNO₃-Na₃PO₄ zwei Maxima bilden: das Silberoxyd- und das Silberphosphat-Maximum, während beim Zusatz von KBr noch ein weiteres Silberbromid-Maximum entsteht. Der Einfluß zugesetzter Salpetersäure wurde systematisch geprüft und die betreffenden p_H-Werte mittels der Glaselektrode bestimmt. Das Silberphosphat-Maximum wird immer bei ungefähr demselben p_H-Wert gebildet. In der Diskussion ist der Charakter der Maxima besprochen. Unter Anwendung kleiner Mengen von Gelatine konnte festgestellt werden, daß das Silberphosphat-Maximum ein Kristallisationsmaximum, während das Silberbromid ein Koagulationsmaximum ist.     

Cobalt(II) Chloride Complex Formation in Acetamide–Calcium Nitrate Tetrahydrate Melts

The absorption spectra of Co(II) chloride complexes, containing variable concentrations of chloride ligand, in a molten mixture of 80 mol% acetamide–20 mol% calcium nitrate tetrahydrate, were studied at 313, 333, 353, and 363 K, in the wavelength range 400-800 nm. The melt contains three possible ligands (CH₃CONH₂, H₂O, and NO₃ ^-) for competition with added chloride ligand. Addition of chloride caused a shift of the absorption maximum of octahedral cobalt(II) nitrate towards lower energies and pronounced changes in the shape of the initial spectrum of cobalt(II) nitrate. The effect of temperature changes on the molar absorption coefficient of the Co(II) species was dependent on the chloride concentration and was attributed to the structural changes occurring in the cobalt(II) species. The STAR and STAR FA programs were applied to identify the complex ionic species and to calculate the stability constants of Co(II) complexes formed in this solvent. The results indicate the highest probability of formation of the following complex species: Co(NO₃)₄ ^2-, Co(NO₃)₂Cl₂ ^2-, and CoCl₄ ^2-. Stability constants of each complex were presented for the equilibria occurring at 313, 333, 353, and 363 K. Distribution of the Co(II) species was also calculated over the ranges of chloride concentration and temperature investigated.     

Migration of radiocesium in a zeolite-solution system

Some properties of natural zeolite from Zaloka gorica, Slovenia, Yugoslavia were investigated to establish its applicability in solidification and for storage purposes of radioactive waste. It was found that this material is a rather good sorber for cesium, with a capacity of about 0.6 meq g^–1. The migration rate of Cs⁺ in a system ion exchanger-aqueous solution was investigated and correlated with the sorption behaviour of cesium in a system. The leaching rate of cesium from concrete containing zeolite was measured.     

A simple procedure for the quantitative microdetermination of rhamnose

Summary A simple spectrophotometric procedure for microdetermination of rhamnose is described. It is based on breakdown of the sugar with sulphuric acid followed by treatment withp-hydroxydiphenyl. The coloured product is measured spectrophotometrically at 560 nm. A linear relationship exists between the amount of rhamnose (10-0g–) and the absorbance. The method is recommended for determination of rhamnose in samples containing rhamnose, different neutral sugars, amino-sugars, sugar alcohols, uronic acids, and muramic acid.

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Zusammenfassung Ein einfaches spektralphotometrisches Verfahren zur Mikrobestimmung von Rhamnose wurde beschrieben. Es beruht auf der Spaltung des Zuckers mit Schwefelsäure und nachfolgender Behandlung mit p-Hydroxydiphenyl. Das gefärbte Reaktionsprodukt wird spektralphotometrisch bei 560 nm gemessen. Die Extinktion steht mit der Rhamnosemenge in linearer Beziehung. Das Verfahren wird für die Rhamnosebestimmung in Proben empfohlen, die verschiedene Neutralzucker, Aminozucker, Zuckeralkohole, Uronsäuren und Muramsäure enthalten.

     

The stability constant ratios of tri-N-octyl amine hydrochloride and bisulphate

The equilibria between the solution of TOA in toluene and mixtures of sulphuric and hydrochloric acid been studied. They were characterized by ratios of stability constants of amine salts formed in the organic phase.