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亚铁测定的关键问题是防止样品分解过程中亚铁被氧化和高铁被还原。近年来提出利用浓硫酸与氢氟酸混合时放出的热量分解样品,较有效地防止亚铁被氧化。此法使用的器皿有铂坩埚和聚四氟乙烯坩埚,我们在聚四氟乙烯坩埚中分解样品,直接用邻菲啰啉光度法测定亚铁,得到很好的结果。用固体硫酸亚铁铵标准物与标样试验,亚铁回收为99.3—99.9%,测定6个日本标样,绝对误差是-0.07—+0.03%,其中1个标样6次测定的精密度和准确度分别是RSD0.28%和0.57%。
The key issue with ferrous determination is the prevention of oxidation of ferrous iron and the reduction of high-speed iron during sample decomposition. In recent years, the use of concentrated sulfuric acid and hydrofluoric acid mixture of heat released when the decomposition samples, more effective in preventing oxidation of ferrous. This method uses a vessel with a platinum crucible and a polytetrafluoroethylene crucible, and we decompose the sample in a polytetrafluoroethylene crucible to directly measure the ferrous using phenanthroline spectrophotometry to obtain good results. Ferrous ammonium sulfate standards with the standard solid samples and standards, ferrous recovery of 99.3-99.9%, 6 Japanese standard samples were measured, the absolute error is -0.07- +0.03%, of which a standard six times the determination of precision And the accuracy is RSD 0.28% and 0.57% respectively.