Identifizierung und quantitative Bestimmung von Alkoxyl sowie ?thylen- und Propylenoxid in monomolekularer und polymerer Form

Summary A method is described for the routine determination of ethylene oxide and propylene oxide, and of C₁-nC₄ alkoxyl groups. It was found that monomeric propylene oxide yields isopropyl iodide and propylene when decomposed by hydriodic acid, but the decomposition of propylene oxide polymers results mainly in the formation of isopropyl iodide (68%) and propionaldehyde (22%): less than 1% of propylene is formed and seven other compounds are also present. Those of the latter that were present in amounts 1% were identified. These results were taken into account in working out the quantitative method.The sample is decomposed in boiling hydriodic acid, volatile products are collected in m-xylene in a cold trap, and ethylene and propylene are measured in a gas burette (nitrometer). 1,1,2-Trichlorethane is added to the m-xylene solution as internal standard, and C₁-nC₄ iodides and propionaldehyde are determined gaschromatographically with Apiezon L on kieselguhr as stationary phase. The time required is 1 hr after the decomposition of the sample is complete, but the working time per sample is less if a series of samples is analysed.

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Meinem verehrten Lehrer, Herrn Prof. Dr. Hans Lieb, zum 80. Geburtstag gewidmet.

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Herrn Dr. Pfab danke ich. für wertvolle Hinweise, Herrn Dr. Noffz für Beratung und anregende Diskussion bei der Einrichtung der Gas-Chromatographie. Die massenspektrometrischen Untersuchungen wurden in dankenswerter Weise von Herrn Dr. Benz, die Papier- und Dünnschicht-Chromatographie von Herrn Dr. Steuerle ausgeführt. Für die gewissenhafte Ausführung der Versuche sei auch an dieser Stelle Herrn Niklas gedankt.