高效液相色谱法分析环己基苯液相氧化体系的组成

Analysis of the cyclohexylbenzene oxidation system by high performance liquid chromatography

采用高效液相色谱法建立了常温下环己基苯(CHB)液相氧化体系中各组分含量的测定方法,利用间接碘量法测定环己基苯氢过氧化物(CHBHP)浓度并以此标定高效液相色谱法,绘制了CHB、CHBHP和1-苯基环己醇(PCHO)3种组分的标准曲线,并用于实际试样的测定。实验结果表明,CHB,PCHO,CHBHP的线性相关系数分别为0.995 5,0.998 2,0.990 7;CHB和PCHO的加标回收率均大于99%,CHBHP的加标回收率接近100%;对实际试样进行了5次平行实验,3种组分的相对标准偏差均不超过0.35%,精密度和准确度高,重复性良好,解决了难以获得CHBHP标准物质的问题。

A high performance liquid chromatography method for the analysis of the composition of cyclohexylbenzene（CHB） oxidation system was established. The concentration of cyclohexylbenzene hydroperoxide（CHBHP） in the system determined by indirect iodometric titration was used to calibrate the high performance liquid chromatography, and the external standard curves of CHB, CHBHP and 1-phenylcyclohexanol（PCHO） were plotted and used for actual samples. The experimental results showed that, the correlation coefficients of the standard curves of CHB, PCHO and CHBHP were 0.995 5, 0.998 2 and 0.990 7, relatively. The recoveries of both CHB and PCHO were more than 99% and the recovery of CHBHP was close to 100%. All the relative standard deviations in repeated measurements 5 times were less than 0.35%. This method is of high precision and good repeatability, which can solve the problem hard to obtain the CHBHP standard substance.