环己酮肟重排反应混合物中游离肟的测定  

Determination of Cyclohexanone Oxime in Beckmann Reaction Rearrangement Mixture

作　　者：陈萍[1] 王艳[2] 段青兵[1] 许定刊[1] 

机构地区：[1]中石化股份有限公司巴陵分公司,岳阳414007 [2]中南大学化学化工学院,长沙410083

出　　处：《化工进展》2004年第8期896-898,共3页Chemical Industry and Engineering Progress

摘　　要：建立了环己酮肟重排反应混合物中游离肟含量的测定方法。研究了重氮化 -偶联反应机理、条件及试剂选择、用量 ,探讨了溴化钾对提高反应速率的作用。该方法灵敏度高、准确性好 ,在最佳实验条件下 ,测定环己酮肟的最小检测限为 0 1mg/L ,变异系数 <1% ,加标回收率为 95 %～ 99%。Diazo coupling reaction spectrophotography has been developed for the determination of cyclohexanone oxime in Beckmann rearrangement mixture sample. The mechanism and condition of diazo coupling reaction have been investigated. In addition,the precision and accuracy of the method were satisfactory. Under the optimum conditions,for cyclohexanone oxime,the detection limit was 0.1?mg/L,the relation standard deviation (RSD) of determinations was below 1%,and the recovery of standard additions method was from 95% to 99%.

关 键 词：BECKMANN重排 环己酮肟 重氮化-偶联反应光度法 

分 类 号：O657.3[理学—分析化学]