Determination of rare earth impurities in high purity uranium by isotope dilution analysis

Summary An isotope dilution method for the determination of rare earth impurities in uranium has been developed and Ce, Nd, Sm, Eu and Gd have been determined in uranium oxide samples. The method involves isotopic dilution with enriched isotopes of the rare earths being measured, followed by the separation of rare earths from uranium. A mass spectrometer with thermionic source was used to determine the relative isotopic abundances in each of these rare earths. All these five elements were analysed selectively by preferential evaporation technique. Trace concentrations down to parts per billion range can be measured with good sensitivity and accuracy.

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Bestimmung von Verunreinigungen an Seltenen Erden in hochreinem Uran durch Isotopenverdünnungsanalyse

Zusammenfassung Eine Isotopenverdünnungsmethode wurde ausgearbeitet zur Bestimmung von Ce, Nd, Sm, Eu und Gd in Uranoxidproben. Das Verfahren umfaßt isotopische Verdünnung mit angereicherten Isotopen der zu bestimmenden Elemente und nachfolgende Abtrennung der Seltenen Erden von Uran. Die relativen Isotopenhäufigkeiten wurden mit Hilfe eines Massenspektrometers mit thermischer Ionenquelle bestimmt. Alle fünf Elemente wurden durch selektive Verdampfung analysiert. Spurenkonzentrationen bis herab zum ppb-Bereich konnten mit guter Empfindlichkeit und Genauigkeit erfaßt werden.

     

The vibrational spectra of maleimide and N-D maleimide

The infrared spectra of maleimide as a vapour (160°C), melt (100°C), oriented polycrystalline film, pellet and when dissolved in various solvents were recorded between 4000 and 400 cm^?1. Also certain spectra in the far infrared region 400-40 cm^?1 were obtained. Raman spectra of the crystalline solid, melt and as a saturated solution in acetonitrile were recorded and semiquantitative polarization measurements carried out. For N-D maleimide infrared and Raman spectra of the solid compound were recorded.The fundamental frequencies have been assigned in terms of C_2v, symmetry on the basis of infrared vapour contours and dichroism of the oriented film as well as on Raman polarization data. A force field was derived for maleimide, by initially transferring force constants from maleic anhydride and subsequent refinement of the force constants. The agreement between observed and calculated frequencies for the in-plane modes was satisfactory whereas certain large discrepancies remained for the out-of-plane vibrations.     

A comparison of two methods for the preparation of 3-Deazapurine ribonucleosides

The reaction of the trimethylsilyl derivative of 4,6-dichloroimidazo[4,5-c]pyridine with 2,3,5-tri-O-benzoyl- D -ribofuranosyl bromide gave four nucleosides-the α- and β-anomers of the 1-isomer and the α- and β-anomers of the 3-isomer (3.9:2.7:1.5:1). In contrast, the fusion reaction of 4,6-dichloroimidazo[4,5-c ]pyridine with 1,2,3,5-tetra-O-acetyl-β- D -ribofuranose gave a high yield of the 1-β-isomer, which was converted to the known 3-deazaadenosine (4-amino-l-β- D -ribofuranosylimidazo[4,5-c]pyridine).     

The weakly bound He-HCCCN complex: high-resolution microwave spectra and intermolecular potential-energy surface

Rotational spectra of the weakly bound He-HCCCN and He-DCCCN van der Waals complexes were observed using a pulsed-nozzle Fourier-transform microwave spectrometer in the 7-26-GHz frequency region. Nuclear quadrupole hyperfine structures due to the 14N and D nuclei (both with nuclear-spin quantum number I = 1) were resolved and assigned. Both strong a and weaker b-type transitions were observed and the assigned transitions were used to fit the parameters of a distortable asymmetric rotor model. The dimers are floppy, near T-shaped complexes. Three intermolecular potential-energy surfaces were calculated using the coupled-cluster method with single and double excitations and noniterative inclusion of triple excitations. Bound-state rotational energy levels supported by these surfaces were determined. The quality of the potential-energy surfaces was assessed by comparing the experimental and calculated transition frequencies and also the corresponding spectroscopic parameters. Simple scaling of the surfaces improved both the transition frequencies and spectroscopic constants. Five other recently reported surfaces [O. Akin-Ojo, R. Bukowski, and K. Szalewicz, J. Chem. Phys. 119, 8379 (2003)], calculated using a variety of methods, and their agreement with spectroscopic properties of He-HCCCN are discussed.     

Direct determination of lead in polluted sea water by carbon-furnace atomic absorption spectrometry

A simple and rapid method is described for the direct determination of lead in polluted sea water by carbon furnace atomic absorption spectrometry. Filtered sea water is diluted (1+1) with'deionised distilled water and ammonium nitrate is added to act as a matrix modifier. Aliquots of this mixture are injected into a tantalum-coated graphite tube in a HGA-2200 furnace atomiser operated under gas-stop conditions. With the standard addi- tion method, a detection limit (20) of 1 μg Pb 1^-1 is achieved. Good agreement between the proposed method and results obtained by anodic stripping voltammetry was achieved for samples taken from the Firth of Forth.     

Localized orbitals in hydrogen bonded systems

The localized molecular orbitals for a variety of hydrogen bonded systems are obtained from their INDO and CNDO/2 wavefunctions. The bonding of these systems is qualitatively discussed in light of the localized orbitals.     

A new entry to the isogeissoschizoid skeleton

[reaction: see text] The tetracyclic isogeissoschizoid skeleton has been prepared by a novel route that involves the ozonolysis and double reductive amination of a cyclopentene, a nickel-catalyzed cyclization, and a late-stage Fischer indole synthesis.     

Development of delta(15)N stratification of NO(3)(-) in soil profiles

New evidence, obtained using a robust method for measuring the delta(15)N of NO(3)(-)-N in soil, is consistent with denitrification being the major determinant in the vertical distribution of NO(3)(-)-delta(15)N in soil profiles. These data also suggest that varying moisture regimes result in different effects of soil NO(3)(-)-N leaching on residual whole soil delta(15)N.     

Compounds with symmetrical tricobalt chains wrapped by dipyridylamide ligands and cyanide or isothiocyanate ions as terminal ligands

Three new linear compounds of the type Co(3)(dpa)(4)X(2), where dpa is the anion of di(2-pyridyl)amine and X is NCS(-) (5), CN(-) (6), and N(CN)(2)(-) (7), have been prepared, and their structures and magnetic behavior have been studied. In all of them, including three different solvates of 5, the Co(3) chains are symmetrical with Co-Co distances of ca. 2.31-2.32 A. The appearance of four lines in the (1)H NMR spectra of the three compounds is also consistent with a symmetrical structure in solution. For all compounds, the magnetic behavior is quite similar with mu(eff) of ca. 1.9-2.0 micro(B) at temperatures between 1.8 and 200 K. As the temperature increases, the effective moments increase gradually, but since saturation is not reached, even at 400 K, the high-spin state cannot be assigned.     

Study of the thermal decomposition of solids in a fluidized bed, III

The influence of the air humidity upon the thermal decomposition of diammonium hydrogen phosphate was studied in a fluidized bed, under isothermal conditions. It was found that the increase of the decomposition rate is influenced directly by the partial pressure of the water vapour in the air, and indirectly by the working temperature. The moisture effect is explained by the salt hydrolysis in the water condensed on the grain surface. The energy of activation of the thermal decomposition decreases when the air humidity increases.

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Zusammenfassung Der Einfluß der Luftfeuchtigkeit auf die thermische Zersetzung des Diammoniumhydrogenphosphats wurde in fluidisiertem Bett unter isothermen Verhältnissen studiert. Die Zunahme der Zersetzungsgeschwindigkeit war direkt proportional dem partialen Wasserdampfdruck in der Luft und indirekt proportional der Arbeitstemperatur. Diese Wirkung wird durch Salzhydrolyse in dem kondensierten Wasser an der Kernoberfläche erklärt. Die Aktivierungsenergie der thermischen Zersetzung nimmt mit zunehmendem Feuchtigkeitsgehalt ab.

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Résumé On a étudié l'influence de l'humidité atmosphérique sur la décomposition thermique de (NH₄)₂HPO₄ en lit fluidisé, en conditions isothermes. La pression partielle de la vapeur d'eau dans l'air intervient directement sur l'augmentation de la vitesse de décomposition et exerce une action indirecte sur la température de travail. On a expliqué l'effet de l'humidité par l'hydrolyse du sel dans l'eau condensée à la surface des grains. La valeur de l'énergie d'activation de la décomposition thermique diminue quand l'humidité atmosphérique augmente.

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