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化学学报
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化学学报 ›› 1963, Vol. 29 ›› Issue (4): 266-276. 上一篇    下一篇

论文

关于落滴法分析重水的研究

金德秋, 張青蓮   

  1. 北京大学化学系
  • 投稿日期:1962-11-30 发布日期:2013-06-03

ON THE DETERMINATION OF DEUTERIUM OXIDE BY MEANS OF THE FALLING DROP METHOD

CHIN TE-CHIU, CHANG TSING-LIEN   

  1. Department of Chemistry, Peking University
  • Received:1962-11-30 Published:2013-06-03

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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%D2O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%D2O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%D2O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.

n-Butyl benzoate is proposed as a new medium for the falling drop method of determination of deuterium oxide in a sample of dilute heavy water.It is suitable for analysis in the concentration range of 0-10.5 mol% D2O at working temperatures 22-33.5℃.A mixed medium composed of n-butyl and iso-butyl benzoate in about 1:1 ratio can be applied to analysis for 0-7 mol% D2O at working temperatures 21.5-26.5℃.iso-Butyl benzoate can be used at 20.5℃ for analysing 0-4 mol% D2O.Calibration curves for these media are shown in Fig.9 and 10* (in Chinese text).The relative error of determination is about 0.1%.