摘要
用吸光光度法分析了丁二烯电化学合成山梨酸的中间产物乙酰氧基己烯酸 (AA)。试验表明 ,AA测定的线性范围为 0～ 10 .1μg/ 10ml ,最大吸收波长λmax为 5 30nm ,摩尔吸光系数为 7 64× 10 4 L·mol- 1·cm- 1。催化剂CuCl最佳用量为 0 .75 μg/ 10ml ,最佳pH为 2 .7～ 3.3,温度条件为 2 7～37℃ ,水解时间为 30min ,样品测定结果满意 ,回收率达 92 .6%～ 10 3.2 %。
An absorptiophotometric method for the determination of acetoxyhexenoic acid (AA), which is an intermediate product in the process of electro synthesis of sorbic acid, was described. In the determination, AA was first hydrolyzed to form sorbic acid at pH 3 and 30℃, through the catalytic action of Cu(Ⅰ)(about 0.7μg). The sorbic acid formed was then oxidized with potassium dichromate in a dilute sulfuric acid medium to form propanedial which was further reacted with thiobarbituric acid to form a red colored complex with its absorption maxima at 530nm. The absorbance of the red complex was directly proportional to the concentration of AA and Beer′s law was kept in the range of 0～10.1μg of AA per 10ml solution, with its molar absorptivity ε =7.64×10 4L·mol -1 ·cm -1 . Interference tests were made and tolerance limits of some of the coexisting ions were found as follows (mg per 10ml solution): OAc - 21.6, Mn(Ⅱ) 4.06,Mn(Ⅲ) 0.17, Recoveries obtained were in the range of 92.6%～103.2%. This method was suitable to be used in the control analysis for electrosynthesis of sorbic acid.
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2002年第4期182-183,共2页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
广东省自然科学基金资助项目 ( 960 0 38)
