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A. Coetzee M. E. Brown D. J. Eve C. A. Strydom 《Journal of Thermal Analysis and Calorimetry》1994,41(2-3):357-385
Both isothermal and programmed temperature experiments have been used to obtain kinetic parameters for the dehydrations and
the decompositions in nitrogen of the mixed metal oxalates: FeCu(ox)2·3H2O, CoCu(ox)2·3H2O and NiCu(ox)2·3.5H2O, [ox=C2O4]. Results are compared with those reported for the thermal decompositions of the individual metal oxalates, Cuox, Coox·2H2O, Niox·2H2O and Feox·2H2O. X-ray photoelectron spectroscopy (XPS) was also used to examinee the individual and the mixed oxalates.
Dehydrations of the mixed oxalates were mainly deceleratory processes with activation energies (80 to 90 kJ·mol−1), similar to those reported for the individual hydrated oxalates. Temperature ranges for dehydration were broadly similar
for all the hydrates studied here (130 to 180°C).
Decompositions of the mixed oxalates were all complex endothermic processes with no obvious resemblance to the exothermic
reaction of Cuox, or the reactions of physical mixtures of the corresponding individual oxalates.
The order of decreasing stability, as indicated by the temperature ranges giving comparable decomposition rates, was NiCu(ox)2>CoCu(ox)2>FeCu(ox)2, which also corresponds to the order of increasing covalency of the Cu−O bonds as shown by XPS.
In celebration of the 60th birthday of Dr. Andrew K. Galwey 相似文献
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M. Krunks I. Oja K. Tõnsuaadu M. Es-Souni M. Gruselle L. Niinistö 《Journal of Thermal Analysis and Calorimetry》2005,80(2):483-488
Thermal decomposition of dried TiO2 gel, obtained by hydrolysing acetylacetonate-modified titanium(IV) isopropoxide, was monitored by simultaneous TG/DTA/EGA-FTIR measurements in dynamic air up to 900°C. XRD and FTIR were employed to identify the solid reaction products. Thermal degradation of the TiO2 gel consists of five distinct mass loss steps, the total mass loss being 43.8%. EGA by FTIR revealed the release of H2O below 120°C; followed by acetone, isopropyl acetate and 1-propanol around 200-300°C, and finally CO and CO2 up to 550°C. Highly exothermic reaction at 410-550°C is caused by the combustion of carbon residues. Crystalline TiO2-anatase is formed around 500°C and TiO2-rutile close to 800°C. 相似文献
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In order to detect small variations in 13C isotopomers concentrations, high sensitivity, accuracy and precision have to be achieved. To assess such criteria, when using 13C NMR, 13C bi-labelled ethanol has been proposed as a molecular probe. Advantage has been taken of the pre-established structural relationship between the peak areas of the 13C NMR spectrum of this molecule, i.e. the ratio of signal areas is set to a fixed value. It is shown that the quality performance, required by quantitative 13C NMR spectroscopy, is not affected by a large reduction of the repetition delay using relaxation reagents. 相似文献
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Terhi Oja Petri Tähtinen Nadine Dreiack Pekka Mäntsälä Jarmo Niemi Mikko Metsä-Ketelä Karel D. Klika 《Tetrahedron: Asymmetry》2012,23(9):670-682
Two new pairs of stereoisomeric alnumycin As, A2 {(2)-(1R,1′RS,4′SR,5′SR)} and A3 {(2)-(1R,1′RS,4′SR,5′RS)}, are described. Similar to alnumycin A1 {(2)-(1R,1′RS,4′RS,5′SR)}, each of these naturally occurring compounds is also a pair of C-1 inverse epimers. The relative configurations of the dioxane ring sidechains were assigned on the basis of 1H NMR NOE contacts and molecular modeling using density functional theory (DFT) at the M06-2X/6-31G(d) level of theory. The absolute configurations of C-1 and the determination of inverse epimeric relationships were achieved by experimental electronic circular dichroism (ECD) measurements, with both aspects confirmed by using the chiral derivatizing agent (CDA) Mosher′s acid chloride {α-methoxy-α-trifluorophenylacetyl chloride (MTPACl)} to effect enantiodifferentiation. The absolute configurations of the dioxane ring using the CDA could only be effected in the case of alnumycin A1, the results of which were in agreement with previous assignments. The dioxane ring conformational mobility and the likely interaction between the MTPA groups coupled with the structural novelty of the diols in the dioxane ring with respect to CDA analysis precluded an absolute configuration assignment for alnumycins A2 and A3 based on empirical comparisons or by computational analysis of through-space NMR shieldings (TSNMRS) emanating from the phenyl groups of the MTPA moieties. 相似文献
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