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The application of TRXRD for thermal analysis is demonstrated using examples of phase transitions, solid-state reactions and high-temperature corrosion. The measuring system produces a series of diffraction patterns, which are evaluated by a difference procedure that a reduces the data to curves comparable to DSC and TG curves and thus suited to kinetic evaluation.  相似文献   
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Summary The formation of -Fe2O3 on Fe3O4 during the oxidation of iron below 570°C occurs very slowly and the scales are so thin that they cannot be detected by microscopy. X-ray diffraction with grazing incidence, equipped with a high temperature device, allows an in situ study of the -Fe2O3 formation even the initial reactions. The formation of -Fe2O3 was studied in isothermal experiments at 400, 450, 500 and 550°C. -Fe2O3 could already be detected at the beginning of the experiments. The difference method, a numerical treatment for kinetic evaluation, yields curves showing the growth of the -Fe2O3 layer. Fitting the parabolic time law to these curves yields the rate constants.  相似文献   
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Time and temperature resolved X-ray diffraction was used for thermal analysis. Series of diffraction patterns were measured, while the samples are heated/cooled stepwise or isothermally with freely selectable temperature programs.The method was applied for the investigation of the phase transitions of ammonium nitrate and HMX (1,3,5,7-tetranitro-1,3,5,7-tetraaza-cyclooctane), when the identification of phases was required. Its capability in the field of kinetics is demonstrated with the isothermal investigation of the solid state reaction of ammonium nitrate with copper oxide and the non-isothermal investigation of the high temperature corrosion of nickel, which was performed by means of a difference procedure. For obtaining structural details peak fitting and Rietveld refinement were applied for the investigation of ammonium nitrate and HMX.We are indebted to Mr. K. O. Hartmann, Mr. H. Fietzek and Mr. H. G. Farr for their assistance during the measurements and for the maintenance of the measuring systems.  相似文献   
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Fast atom bombardment, combined with high-energy collision-induced tandem mass spectrometry, has been used to investigate gas-phase metal-ion interactions with captopril, enalaprilat and lisinopril, all angiotensin-converting enzyme inhibitors.Suggestions for the location of metal-binding sites are presented. For captopril, metal binding occurs most likely at both the sulphur and the nitrogen atom. For enalaprilat and lisinopril, binding preferably occurs at the amine nitrogen. Copyright 1999 John Wiley & Sons, Ltd.  相似文献   
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