真空蒸留法によるナトリウム中の酸素の定量

概要

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A vacuum distillation method is described for the determination of oxygen in sodium. Water absorbed on inner surface of distillation vessel causes high blank values. In order to remove the water, about 1g of sodium in a nickel crucible is distilled prior to the analysis of actual sample. After the empty nickel crucible is removed from the distillation vessel in an inert atmosphere glove box, a stainless steel crucible containing 35g of sodium sample is placed in the vessel and the vessel is taken out of the glove box.<BR>Following the evacuation of the vessel, the crucible is heated at 350°C under vacuum. When the distillation is complete and the vessel has cooled, argon is allowed to enter into the vessel in the glove box, and the crucible is removed through a glass tube to avoid sodium contamination. Residue in the crucible is dissolved in water and titrated with 0.001<I>N</I> sulfuric acid. From the amount of alkali in the residue, the corresponding oxygen can be determined. The results are in good agreement with those obtained by the amalgamation method.
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