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Cation deficient spinels NixMn3−x3δ/4O4+δ (0≤x≤1) have been prepared by thermal decomposition of mixed oxalates Nix/3Mn(3−x)/3(C2O4nH2O in air at 623 K. They have been characterised by temperature programmed reduction (TPR) under H2, the reaction being followed by gravimetric and powder X-ray diffraction measurements. It has been shown that TPR proceeds in several steps. The first steps correspond to the loss of nonstoichiometric oxygen leading to the formation of a stoichiometric oxide. During the following stages the manganese cations are reduced, causing the spinel structure to be destroyed, and the formation of solid solution of NiO in a cubic MnO. Subsequently, Ni2+ cations undergo a reduction to metallic nickel, and, finally, a mixture of nonstoichiometric MnO1−δ and metallic nickel is formed. These oxides contain a high level of vacancies which vary with the nickel content with a maximum of δ≈1 near x=0.6. This nonstoichiometry is ascribed both to the presence of Ni3+ and excess of Mn4+.  相似文献   
73.
In comparison with direct measurements of unsaturated hydraulic conductivity, the methods of calculations from the moisture retention curve are attractive for their fast and simple use and low cost. These are the main reasons for their increasing use, mainly in spatial variability studies. On the other hand, it is known that their applicability is limited. The possibility of the use of the retention curve to indirectly determine hydraulic conductivities is analyzed as follows. The theoretical derivation of the relationK(h) – (h) is briefly discussed with regards to potential sources of inaccuracy. The sensitivity of the algorithm forK(h) calculation is studied as a response to possible inaccuracies in the retention curve determination. Conclusions about the usability of calculated hydraulic conductivities are drawn.  相似文献   
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Doublet mass measurements of the isobars28Si3 and12C7 are performed by use of a Penning trap mass spectrometer and the Fourier transform ion cyclotron resonance (FT-ICR). The carbon and silicon cluster ions are produced by laser ablation. Results of these preliminary measurements are presented.  相似文献   
76.
Photoirradiated in presence of acetophenone, benzo[b]selenophene and its 3-methyl derivative add to dimethyl acetylenedicarboxylate. In each ease, the primary reaction product is unstable and has not been isolated. Photoexeited in its triplet state (the energy of which is in the neighbourhood of 69 kcalmole) benzo[b]selenophene and its 2- and 3-methyl, 2,3 dimethyl, 3 acetoxy and 2-methyl-3-acetoxy derivatives add to 1,2 dichloroethylene leading to cyclobutanes. Neither cyclo-addition occurs in absence of photosensitiser. Single-crystal X-ray analysis gave the structures of the two adducts of 3-acetoxybenzo[b]selenophene with trans-1,2-dichloroethylene. In both compounds the chlorine atoms are trans.  相似文献   
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