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[目的]研究操作简便、易于收集的氰制备方法及在顶空的稳定性,并建立其标定方法,为新熏蒸剂氰的研制与开发提供依据。[方法]以饱和氰化钾和硫酸铜溶液为试剂,在密闭系统中反应制备并收集氰,用带气体密度电平的气相色谱仪标定氰的纯度。[结果]在90~95℃条件下可制备纯度(体积分数)91%~93%氰,制备后4 h氰在溶液顶空的降解率小于1%。在给定的色谱条件下,空气、二氧化碳和氰能完全分离,氰保留时间为2.35 min。[结论]该方法设备简单,操作方便,易于推广应用。
[Objective] The study aimed to study the preparation method of cyanide and its stability in headspace, which is easy to operate and easy to collect and establish its calibration method to provide the basis for the research and development of new fumigant cyanide. [Method] Saturated potassium cyanide and cupric sulfate solution were used as reagents to react and prepare cyanide in a closed system. The purity of cyanide was calibrated by gas chromatography with gas density level. [Result] The purity (volume fraction) of 91% ~ 93% cyanide was prepared at 90 ~ 95 ℃. The degradation rate of cyanide in solution headspace was less than 1% after 4 h. Under the given chromatographic conditions, air, carbon dioxide and cyanide can be completely separated with a retention time of 2.35 min. [Conclusion] This method has the advantages of simple equipment, convenient operation and easy popularization and application.