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Abstract

Thermal behaviour of hexaamminenickel(II) nitrate and tris(ethylenediamine)nickel(II) nitrate have been investigated by means of simultaneous thermogravimetry/DTA coupled online with mass spectral (MS) studies and temperature resolved X-ray diffraction (TR-XRD) techniques under inert atmospheric condition. Both the complexes produce highly exothermic reactions during heating due to the oxidation of the evolved ammonia or ethylenediamine by the decomposition products of Ni(NO3)2. Evolved gas analysis by MS studies detected fragments like NH2 and NH ions with weak intensity. The decomposition of nitrate group generates N, N2, NO, O2 and N2O species. Ethylenediamine (m/z 60) is fragmented to H2 (m/z 2), N (m/z 14), NH3 (m/z 17) and CH2=CH2/N2 (m/z 28) species. The formation of the intermediates was monitored by in situ TR-XRD. The residue of thermal decomposition for both the complexes was found to be crystalline NiO in the nano range.

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Abstract

Detailed investigation on the thermal behaviour of hexaamminenickel(II) chloride and hexaamminenickel(II) bromide has been carried out by means of simultaneous TG/DTA coupled online with mass spectroscopy (TG-MS) and temperature-resolved X-ray diffraction (TR-XRD). Evolved gas analyses by TG-MS revealed the presence of NH2, NH, N2 and H2 fragments in addition to ammonia during the deamination process. These transient species resulted due to the fragmentation of the evolved ammonia during pyrolysis. The intermediates formed during the thermal deamination stages were monitored by in situ TR-XRD. The final product of the decomposition was found to be nano size metallic nickel in both cases. Morphology of the complexes, intermediates and the residue formed at various decomposition stages was analysed by scanning electron microscope (SEM). Kinetic analyses using isoconversional method for deamination and dehalogenation reaction show that the activation energies vary with the extent of conversion, indicating the multi-step nature of these solid state decomposition reactions.

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Abstract  

Anion exchange separation of250Fm (30 m) synthesized by the12C+242Pu and16O+238U reactions has been investigated with mineral acid-methyl alcohol mixed media at elevated temperature. Fermium was chromatographically separated from the other transplutonium elements, the target materials and an Al catcher foil by anion exchange with mixtures of nitric acid and methyl alcohol. By use of the mixed media of hydrochloric acid and methyl alcohol, Fm together with Cf was separated from Al, Am, Cm, Pu, U and major fission products. The separation systems are suitable for rapid separation and immediate alpha-counting source preparation of Fm.

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Abstract  

Fe-57 Mössbauer spectra of silica-supported Pd–Fe bimetallic catalysts show remarkable changes with varying Fe/Pd atomic ratios. From the spectra, the main Fe-component is estimated as highly dispersed Fe in the Fe/Pd range of 0.05–0.3 and -Fe ensemble and Fe–Pd intermetallics in the Fe/Pd range above 0.3. It is suggested that the chemical state of iron is associated with the catalytic performance in effective CO–H2 conversion to methanol.

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Journal of Radioanalytical and Nuclear Chemistry
Authors:
H. Natsume
,
H. Umezawa
,
T. Suzuki
,
F. Ichikawa
,
T. Sato
,
S. Baba
, and
H. Amano

Abstract  

A scheme for the sequential separation of fission products has been developed on the basis of ion-exchange techniques. It consists of a main cation-exchange process for group separation and subsidiary processes of cation or anion exchange for further separations or purifications of the individual fission products. By the present method, Zn, Rb, Sr, Y, (Zr), Mo, Pd, Cd, Te, Cs, Ba, La, Ce, Pr, Nd, Pm, Sm, Eu and Tb can be separated simultaneously from an irradiated uranium sample. Of these, alkali, alkaline earth and rare earth metal ions are separated quantitatively. A polarographic method was applied to determine the recoveries of Zn, Mo, Pd, Cd and Te, which were not separated quantitatively.

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Journal of Radioanalytical and Nuclear Chemistry
Authors:
T. Maruyama
,
D. Kaji
,
T. Kaneko
,
S. Goto
,
K. Tsukada
,
H. Haba
,
M. Asai
,
S. Ichikawa
,
Y. Nagame
, and
H. Kudo

Abstract  

Rapid chemical separation of berkelium is essential in order to measure the unknown isotope 252Bk. An anion exchange system of mineral acid and methanol was examined. An elution curve of Bk was obtained using 250Bk produced by the 248Cm+18O system and the 251Bk activity could be measured in the preliminary experiments. The whole chemical separation was completed within 30 minutes.

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Journal of Radioanalytical and Nuclear Chemistry
Authors:
A. Toyoshima
,
K. Tsukada
,
H. Haba
,
M. Asai
,
S. Goto
,
K. Akiyama
,
I. Nishinaka
,
S. Ichikawa
,
Y. Nagame
, and
A. Shinohara

Abstract  

The anion exchange behavior of 255No produced by the 248Cm(12C,5n) reaction has been investigated in 11.5M HCl, 4M HCl and 8M HNO3 to deduce the behavior of 'primordial 257No' produced via 248Cm(18O,5n)261Rf 257No before anion exchange separation in the 261Rf experiment. It was found that 255No is mostly eluted from the anion exchange column with these solutions. The contribution of 'primordial 257No' to the -decay events of 261Rf in the 261Rf experiment was evaluated based on the present results.

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Journal of Radioanalytical and Nuclear Chemistry
Authors:
Y. Zhao
,
T. Ohtsuki
,
Y. Nishinaka
,
K. Tsukada
,
S. Ichikawa
,
H. Ikezoe
,
Y. Hatuskawa
,
K. Hata
,
M. Tanikawa
,
Z. Qin
,
K. Sueki
,
Y. Oura
,
H. Kudo
, and
H. Nakahara

Abstract  

Two kinds of scission configurations for certain mass division have been verified by the accurate measurements of fragment velocities in protoninduced fission of actinides: compact and elongated scission configurations. A correlation between the binary scission configurations and mass yield distributions reveals that elongated scission configurations are associated with the symmetric mass distribution and compact scission configurations with the asymmetric mass distribution. The elongation properties of nuclei at scission in a wide range of actinides fissions are studied. The results suggest that the compact and the elongated scission configurations in light actinides fission smoothly change to the scission properties of the symmetric and the asymmetic modes in heavy actinides fission.

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Journal of Radioanalytical and Nuclear Chemistry
Authors:
T. Sekine
,
S. Ichikawa
,
A. Osa
,
M. Koizumi
,
H. Iimura
,
K. Tsukada
,
I. Nishinaka
,
Y. Hatsukawa
,
Y. Nagame
,
M. Asai
,
Y. Kojima
,
T. Hirose
,
M. Shibata
,
H. Yamamoto
, and
K. Kawade

Abstract  

Studies on the decay of unstable nuclei using the two on-line isotope separators of JAERI are reviewed for the past five years. With the previously established ion-source technique using mono-oxide ion formation in a thermal ion source, the new nuclides125Pr and127Pr have been identified in heavy-ion fusion residues. Further, with a newly developed gas-jet coupled thermal ion source, the new nuclides166Tb,165Gd,161Sm and236Am have been identified by bombarding238U and235U targets with a proton or6Li beam. Other studies, including off-line experiments, by decay spectroscopy, laser spectroscopy and Mössbauer spectroscopy are described.

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Journal of Radioanalytical and Nuclear Chemistry
Authors:
S. Goto
,
D. Kaji
,
I. Nishinaka
,
Y. Nagame
,
S. Ichikawa
,
K. Tsukada
,
M. Asai
,
H. Haba
,
S. Mitsuoka
,
K. Nishio
,
M. Sakama
,
Y. Zhao
,
K. Sueki
,
K. Tanikawa
,
K. Takamiya
,
H. Kudo
, and
H. Nakahara

Abstract  

To study the correlation between fragment mass distributions and shell structures of fission fragments, fragment mass and energy distributions in proton-induced fission of 232Th and uranium isotopes, 233,235,238U, were precisely measured using a double-TOF method. It was found that the lighter side of the heavier wing of asymmetric mass distributions shifts to larger fragment mass number corresponding to the N/Z value of the fissioning nucleus. The results are explained qualitatively by the change of the most probable mass number of fission fragments of Z = 50 proton-shell.

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