卡尔·费休容量法测定环己酮氨肟化反应体系的水分含量  

Karl Fischer volumetric determination of water content in cyclohexanone ammoximation reaction system

作　　者：王雪 WANG Xue(Analysis and Test Center of SINOPEC Baling Petrochemical Co.,Ltd,Yueyang 414007)

机构地区：[1]中石化巴陵石油化工有限公司分析检验中心,湖南岳阳414007

出　　处：《合成纤维工业》2021年第4期89-93,共5页China Synthetic Fiber Industry

摘　　要：采用卡尔·费休容量法测定环己酮氨肟化反应体系的水分含量(W),探讨了卡尔·费休试剂的种类、浓度、试样中的杂质组分、仪器操作条件对测定试样中的W的影响。结果表明:选择KFR-04型卡尔·费休醛酮专用试剂A液、B液能消除环己酮的干扰,且反应体系中的其他主要组分叔丁醇、环己酮肟、环己醇、氨无明显干扰;在卡尔·费休醛酮专用试剂B液浓度为5 g/L、进样量30μL、仪器滴定速率设置“Optimal”、初始漂移值为20μL/min的条件下测定环己酮氨肟化反应体系的W,其加标回收率为97.54%~103.06%,相对标准偏差为0.092%~0.110%。The water content(W)of cyclohexanone ammoximation reaction system was determined by Karl Fischer volumetric method.The effects of the type and concentration of Karl Fischer reagents,impurity components in samples and instrument operation conditions on the determination of W were discussed.The results showed that the interference of cyclohexanone could be eliminated by KFR-04 Karl Fischer aldehyde ketone special reagent A and B,and there was no obvious interference of other main components in the reaction system,such as tert butyl alcohol,cyclohexanone oxime,cyclohexanol and ammonia;and the standard addition recovery rate was 97.54%-103.06%and the relative standard deviation was 0.092%-0.110%when W of cyclohexanone ammoximation reaction system was determined under the conditions as follows:Karl Fischer aldehyde ketone special reagent B concentration 5 g/L,injection volume 30μL,titration rate set as"Optimal",initial drift value 20μL/min.

关 键 词：卡尔·费休容量法 环己酮 氨肟化反应体系 水分含量 醛酮试剂 测定 

分 类 号：TQ207+.2[化学工程—有机化工]