改良型燃焼フラスコを用いる有機ハロゲンおよびイオウの微量定量 : フラスコ燃焼法による有機元素分析(第1報)

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Analytical procedures could be very conveniently and rapidly performed by a method using a combustion flask with joint equipped with a measuring pipet, stopper cock, oxygen introduction pipe, washing pipe, washing effusive hole, platinum lead wire, platinum coil, and platinum, or quartz basket, etc. In quantitative analysis with this apparatus, it is desired that the volume of absorption fluid be made as small as possible. For this purpose, the interior of the flask is washed with distilled water, which is then removed completely by shaking the flask several times, and thereafter placing an absorbent therein. In the analysis of iodine, a satisfactory result was obtained by using sodium oxide in place of hydrogen peroxide. After sample combustion, the flask was allowed to stand, without shaking, in ice water for about 1 minute. The inner surface of the flask, cock, and basket could be rinsed automatically with the fluid aspirated by reduced pressure in the flask. Thus, titration could be performed without transferringthe fluid to other vessels. The titration was carried out with 0.005N Hg(NO3)2 for Cl, Br, and I; with 0.01N Th (NO3)4 for F; and with 0.01N Ba(CH3COO)2 for S. It took only 67 minutes to complete the analysis, excluding the time required for weighing the sample.
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