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本文詳細研究重水分析的落滴法,主要結果有: 1.提出苯甲酸正丁酯作为落滴法分析稀重水的新介貭。用多温法可在22—33.5°間适用于分析0—10.5克分子％D_2O浓度范围。苯甲酸正异丁酯(約1:1)混合介貭在21.5—26.5°间适用于分析0—7克分子％D_2O浓度范围。在这些介貭中的工作曲綫(图10;273頁脚註)已都制訂。苯甲酸异丁酯在20.5°时适用于分析0—4克分子％D_2O浓度范围。測定的相对誤差为±0.1％。 2.对上述三种介貭和邻氟甲苯各作500滴稳定性試驗,它們到达稳定状态的前期不相同。用預飽和法可消除这一“前期”效应。 3.邻氟甲苯是一种稳定的介貭,不同于Krell等的意見而与Hytten等的观察一致。 4.曾观察不同体积的前滴所引起的管端余液体积的大小,証明用較細的管端:約1.4毫米外径,可減小余液效应,致使計量为8.00微升大小的后滴的降落时間讀数,能恆定在±0.1％以內。
In this paper, the drop-dropping method of heavy water analysis is studied in detail. The main results are as follows: 1. The n-butyl benzoate is proposed as a new medium for the analysis of dilute water by dropping-drop method. The multi-temperature method is suitable for the analysis of the concentration range of 0-10.5 mol% D 2 O between 22-33.5 °. N-Butyl benzoate (ca. 1: 1) Mixing medium is suitable for the analysis of a range of 0-7 mol% D 2 O between 21.5-26.5 °. The working curves in these profiles (Figure 10; footer to page 273) have been formulated. Isobutyl benzoate is suitable for the analysis of 0-4 mol% D_2O concentration range at 20.5 °. The relative error of the measurement is ± 0.1%. 2. For each of the above three intermediates and o-fluorotoluene for 500 drops of stability test, they reach a steady state of the previous period is not the same. Pre-saturation method to eliminate this “early” effect. 3. O-fluorotoluene is a stable medium, different from the observations of Krell et al., In line with the observations of Hytten et al. 4. It was observed that the volume of tubing remaining volume caused by the different volumes of the first droplet proves that with a thinner tube end: about 1.4mm OD, the residual fluid effect can be reduced, resulting in a metered volume of 8.00μL Drop landing time reading, can be constant within ± 0.1%.