四塩化チタン中の炭素と水素の同時定量法

概要

論文の詳細を見る
A dry method of simultaneous determination of carbon and hydrogen in titanium tetrachloride has been established. The merits of an appratus (Fig. 1) devised are mentioned as follows: (1) A sampling vessel of a new type is devised for a complete avoidance of atmospheric contamination. (2) A trap (Table I and II) is set to prevent low boiling substances for escaping out of the system during the exchanging of atmospheres. (3) By inserting a quartz spiral, a complete oxidation of sample is made possible without any disturbance. (4) To remove a large amount of chlorine evolved during the oxidation of sample, a silver wire is employed.<BR>By using the apparatus, analytical conditions of standard titanium tetrachloride with additions of various known amounts of compounds containing carbon and hydrogen have been investigated. In the process of the method, 0.5 m<I>l</I> sample is placed on a boat, vaporized for 10 min in the atmosphere of oxygen and oxidized by heating at 11001200°C. After the gas generated by combustion of the sample is driven out for 20min, the content of carbon and hydrogen are determined by microgravimetric method. This method can be applied for analysis of total carbon and total hydrogen in titanium tetrachloride with 100 % recovery. Its accuracy was within 9% in terms of variation coefficient for both carbon and hydrogen (Table III) and the lower limit of determination was 0.001%.
社団法人日本分析化学会の論文