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Synthesis, freeze-drying and characterization of 57Fe(III) acetate

机译:乙酸57Fe(III)的合成,冷冻干燥和表征

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摘要

Iron(III) acetate was synthesized by the reflux method using iron enriched in the 57Fe isotope and the compound processed by freeze-drying. The as-synthesized and freeze-dried acetates were characterized regarding their structural, thermal, vibrational and hyperfine properties. Similar diffractometric and spectroscopic results were found for both materials and also for an industrial acetate made with natural iron. However, the microstructures differed: the as-synthesized compound showed flake morphology with micrometric dimensions, whereas the freeze-dried showed flake morphology with sub-micrometric dimensions. The activation energies for thermal decomposition, calculated from the exothermic events occurring in differential scanning calorimetry measurements, were 100.9 kJ/mol (as-synthesized) and 114.7 kJ/mol (freeze-dried).
机译:乙酸铁(III)通过回流法使用富含57Fe同位素的铁合成,并通过冷冻干燥处理该化合物。合成后的乙酸盐和冻干的乙酸盐的结构,热,振动和超细特性均得到了表征。对于两种材料以及由天然铁制成的工业乙酸盐,都发现了相似的衍射和光谱结果。但是,微观结构不同:合成后的化合物显示出具有微米级尺寸的片状形态,而冷冻干燥的显示出具有亚微米级尺寸的片状形态。根据在差示扫描量热法测量中发生的放热事件计算出的热分解活化能分别为100.9 kJ / mol(合成后)和114.7 kJ / mol(冷冻干燥)。

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