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本文研究了四氟化铀中氟化铀酰的极谱测定法.以10%甲醇溶液浸取四氟化铀中的可溶性氟化铀酰,然后以1M HClO_4-0.1M ACl_3为底液,用极谱法测定浸取液中的六价铀。在此底液中,六价铀极谱波波形良好,其极限电流仅受扩散控制。氟化铀酰在10%甲醇溶液中的溶解度较大,四氟化铀的溶解度则较小。在空气中浸取一小时,四氟化铀中六价铀浓度无显著提高。铬、钨、钛、铈、铁等离子对测定无干扰。钒和钼离子的浓度分别小于5和1微克/毫升时,对测定也无显著影响。应用本法测定了氟化铀酰含量为1.36%的四氟化铀试样,其标准偏差为±0.069%,若可信度为95%,测定误差在0.14%范围内。本法与奈普法的测定结果一致。
In this paper, the polarographic determination of uranyl fluoride in uranium tetrafluoride was studied.The soluble uranyl fluoride in uranium tetrafluoride was leached with 10% methanol solution, and then with 1M HClO_4-0.1M ACl_3 as the bottom liquid, Determination of Hexavalent Uranium in Leaching Solution by Polarographic Method. At this end, the hexavalent uranium polarographic waveform is well-formed and its limiting current is controlled only by diffusion. The solubility of uranyl fluoride in 10% methanol solution is larger and the solubility of uranium tetrafluoride is smaller. After leaching in the air for one hour, there was no significant increase in the concentration of hexavalent uranium in uranium tetrafluoride. Chromium, tungsten, titanium, cerium, iron plasma on the determination of interference. The concentrations of vanadium and molybdenum ions of less than 5 and 1 μg / ml, respectively, had no significant effect on the assay. The method has been applied to the determination of uranium tetrafluoride samples with uranyl fluoride content of 1.36% with a standard deviation of ± 0.069%. If the confidence level is 95%, the determination error is within 0.14%. This method is consistent with the results of Naipu test.