Analysis of chlorine-oxygen gas mixtures

Analysis of chlorine-oxygen gas mixtures
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氯氧气体混合物的分析

DOI:
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发表时间:
1987
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影响因子:
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通讯作者:
A. Cook
A. Cook
中科院分区:
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文献类型:
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作者:
A. Mills;A. Cook

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设计了一种简单、廉价的方法,用于使用流动系统分析氯氧气体混合物,即在该系统中,将待测气体样品注入混合室,并通过惰性载气 (N2) 吹扫至氯气捕集器,然后进入氧气检测器。发现注入样品中存在的任何氯气(低至约 10 µl)会被直接放置在混合室后面的捕集溶液中存在的碘化物定量减少。然后通过分光光度法测定由于该反应形成的三碘化物的量。通过碘化物捕集器去除氯,然后使用氧膜极谱检测器 (O2-MPD) 检测样品中存在的任何氧气(低至约 20 µl)。此外,还开发了一种用于原位产生准确已知量氯气的化学系统,并使用流动系统演示了其可应用的广泛范围(10 ml-10 µl)。在化学系统中,将准确已知数量的 CeIV 离子注入浓盐水溶液 (2 mol l-1) 中,并添加少量热激活的 RuO2.xH2O。热活化的 RuO2.xH2O 充当氧化还原催化剂,通过 2Ce4++ 2Cl–→ 2Ce3++ Cl2 反应,氯离子定量还原注入的 CeIV 离子。有趣的是,在没有盐水的情况下,该化学系统将通过水定量还原注入的CeIV离子来产生氧气,即4Ce4++ 2H2O → 4Ce3++ 4H++ O2。因此,它还可用于产生准确已知量的氧气和氯。该化学系统提供了一种校准流量系统的有用方法,以准确测定少量氯(<1 ml)。本文还讨论了与处理少量氯气以进行校准相关的问题。
A simple, inexpensive method has been devised for the analysis of chlorine-oxygen gas mixtures using a flow system, i.e., a system in which the gas sample under test is injected into a mixing chamber and swept out by an inert carrier gas (N2) to a chlorine trap and then an oxygen detector. Any chlorine gas (down to ca. 10 µl) present in the injected sample was found to be reduced quantitatively by the iodide present in the trap solution placed directly after the mixing chamber. The amount of triiodide formed as a result of this reaction was then determined spectrophotometrically. Removal of the chlorine by the iodide trap allowed any oxygen (down to ca. 20 µl) present in the sample then to be detected using an oxygen membrane polarographic detector (O2-MPD). In addition, a chemical system for the in situ generation of accurately known amounts of chlorine gas was developed and the wide range over which it can be applied (10 ml-10 µl) was demonstrated using the flow system. In the chemical system, accurately known amounts of CeIV ions were injected into a strong brine solution (2 mol l–1) to which a small amount of thermally activated RuO2.xH2O had been added. The thermally activated RuO2.xH2O acted as a redox catalyst for the quantitative reduction of the injected CeIV ions by the chloride ions via the reaction 2Ce4++ 2Cl–→ 2Ce3++ Cl2. Interestingly, in the absence of brine, this chemical system will generate oxygen via the quantitative reduction of the injected CeIV ions by water, i.e., 4Ce4++ 2H2O → 4Ce3++ 4H++ O2. As a result, it can also be used to generate accurately known amounts of oxygen and chlorine. This chemical system provided a useful method for calibrating the flow system for the accurate determination of small amounts of chlorine (<1 ml). The problems associated with handling small amounts of chlorine gas for calibration purposes are also discussed in the paper.