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采用高温熔融和硫酸冒烟处理样品,用分光光度法联测法测定铝电解质中二氧化硅和三氧化二铁含量的方法。在HNO3介质中,用硅钼蓝光度法测铝电解质中SiO2,ε700=2.1×104L.mol-1.cm-1。实验表明,SiO2的浓度在0~1.75μg/mL范围内时符合比尔定律。在HAc-NaAc(Ph=4.9)的介质中,用邻菲啰啉光度法测铝电解质中Fe2O3,ε510=1.1×104L.mol-1.cm-1。实验表明,Fe2O3的在0.0~2.5μg/mL范围内时符合比尔定律。SiO2加标回收率为98%~104%,Fe2O3加标回收率为94.8%~104.8%。本方法测定铝电解质中的SiO2和Fe2O3具有选择性好、灵敏度高和准确可靠等特点,并获得了较满意的分析结果,为更加科学的调整电解质分子比提供了基础数据。
The samples were treated with high-temperature melting and sulfuric acid smoke, and the content of silica and ferric oxide in the aluminum electrolyte was determined by spectrophotometry. In the HNO3 medium, Si02 was measured in the electrolyte of aluminum by silico-molybdenum blue spectrophotometry with ε700 = 2.1 × 104L.mol-1.cm-1. Experiments show that the concentration of SiO2 in the range of 0 ~ 1.75μg / mL in line with Bill’s law. In the medium of HAc-NaAc (Ph = 4.9), Fe2O3 and ε510 = 1.1 × 104L.mol-1.cm-1 were determined by spectrophotometry of phenanthroline. Experiments show that, Fe2O3 in the range of 0.0 ~ 2.5μg / mL in line with Bill’s law. The spiked recoveries of SiO2 were 98% -104%, and the spiked recoveries of Fe2O3 were 94.8% -104.8%. The method has the advantages of good selectivity, high sensitivity, accuracy and reliability in the determination of SiO2 and Fe2O3 in the aluminum electrolyte. The obtained analytical results are satisfactory and provide the basic data for more scientific adjustment of the molecular ratio of the electrolyte.