[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。
In order to provide the basis for the study and development of new fumigant cyanogen,the preparation method with simple operation and convenient collection and the stability of cyanogen were studied and the calibration was also developped.[Methods] Cyanogen was prepared and collected with saturated solution of KCN and CuSO4 as the reagent in the closed system.Its purity was analyzed using gas chromatograph with gas density balance.[Results] The purity of cyanogen prepared at 90-95 °C was 91-93%(by vol).Its degradation was less than 1%(by vol) in the headspace over the solution 4 h after prepared.Air,carbon dioxide and cyanogen could be separated under the given condition of gas chromatograph,and retention time of cyanogen was 2.35 min.[Conclusions] The method was simple,convenient and worthwhile of spreading widely.