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本文提出了一个纯氧化镧的光镨直接测定方法,即氧—氩气氛激发直流电弧粉末法。十四个杂质元素测定下限分别为:(PPm) CeO_2 7、Pr_6O_(11) 10、Nd_2O_3 5、Sm_2O_3 1、Eu_2O_3 0.5、Gd_2O_3 5、Tb_4O_7 10、Dy_2O_3 1、Ho_2O_3 1、Er_2O_3 1、Tm_2O_3 1、Yb_2O_3 0.1、Lu_2O_3 10、Y_2O_3 3。经五十一条镨线单次测定,方法百分相对均方偏差为±10—±20%。以P350为萃取剂,溴酸钾氧化萃取,微酸性硝酸反萃进行富集。提出了一个简捷的化学富集方法。试样的化学处理可在三—四小时内完成,富集倍数控制在5—15倍,与上述直测方法衔接,以十倍计每个杂质测定下限提高一个数量级。微克级加料试验回收率90—110%。上述方法能满足高纯及纯氧化镧的分析和工艺流程中的控制分析。与国内已发表的方法相比,具有准确、简便、灵敏度高等优点。
In this paper, a direct spectrophotometric method for the determination of lanthanum oxide is proposed, that is, the oxygen-argon atmosphere excites the DC arc powder method. The lower limits of determination of fourteen impurity elements are: (PPm) CeO 2 7, Pr 6 O 11, Nd 2 O 3 5, Sm 2 O 3 1, Eu 2 O 3 0.5, Gd 2 O 3 5, Tb 4 O 7 10, Dy 2 O 3 1, Ho 2 O 3 1, Er 2 O 3 1, Tm 2 O 3 1, Yb 2 O 3 0.1, Lu_2O_3 10, Y_2O_3 3. After a single line of fifty-one praseodymium line method, the method of relative percentage deviation of ± 10% ± 20%. P350 as extractant, potassium bromate oxidation extraction, slightly acidic nitric acid stripping enrichment. A simple method of chemical enrichment is proposed. The chemical treatment of the sample can be completed in three to four hours, the enrichment factor is controlled at 5-15 times, and with the direct measurement method described above, the lower limit of each impurity is increased by one order of magnitude by an order of magnitude. Micrometer feed test recovery 90-110%. The above method can meet the analysis and control analysis of high purity and pure lanthanum oxide in the process flow. Compared with the published methods in China, it has the advantages of accuracy, simplicity and sensitivity.