有機化合物中のイオウの微量定量法

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In order to improve the silver absorption method for the determination of sulfur in organic compounds silver wool made by elctrolysis was used. The sample was burned in the combustion part using an oxygen stream. The rate was 1525 ml per minute. D in Fig. 1 is a movable furnace and its rate of travel is 4.7 mm per minute. The silver wool mentioned above was filled into an absorption tube with a ground-glass joint (Fig. 2), and was heated to 480500°C. A gas stream was passed through the tube, and the sulfur oxide combined with the silver, and a silver sulfate was formed quantitatively. The sulfate was extracted with hot water after a contact period of 2 minutes, and this silver wool was washed completely using 15 ml of hot water into a 100 ml beaker. To the solution were added 2 ml of 4 N nitric acid and 0.5 ml of 40% ferric amonium sulfate solution as an indicator. This solution was then titrated with 0.01 N ammonium-thiocyanate solution, and agitated by a magnetic stirrer. This method is precise and accurate as shown in Table 3 and 4. An acceptable range of this method is shown in Fig. 3. Some conditions were also studied, and it was found that the temperature of the absorption tube changed to 420430°C, and that accurate resulte could be obtained when more than 2 grams of silver wool were used, as is shown in Table 2. An acceptable range of this method is compared with that of the old method using silver wire of 0.06 mm diameter (Fig. 4). This method can be extended to the range of a minute quantity of sulfur such as 0.011%.
社団法人日本分析化学会の論文

有機化合物中のイオウの微量定量法

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