高效液相色谱法测定硝基苯催化加氢的反应产物

Determination of the Reaction Product of Catalytic Hydrogenation of Nitrobenzene by High Performance Liquid Chromatography

采用高效液相色谱和紫外检测器对硝基苯催化加氢的反应产物进行检测。硝基苯催化加氢后的反应液用0.45μm的微孔过滤膜(水系)进行过滤,然后用甲醇稀释后进样。实验利用直接与已知标准物对照的保留值定性方法进行定性分析,采用外标法进行定量分析,通过实验求得了硝基苯、苯胺和对氨基苯酚的线性回归方程,相关系数分别为0.998 60、.999 8和0.999 9,方法检测限分别为2.0、20.0、21.0 mg/L,三者的回收率分别为97.6%、97.5%和98.1%,以相对标准偏差表示的精密度分别为0.62、0.77和0.36。所建立的方法迅速准确简单,不需要对样品进行预处理,实验结果比较令人满意。

The reaction product of catalytic hydrogenation of nitrobenzene was determined by high performance liquid chromatography and UV detection.The reaction solution of catalytic hydrogenation of nitrobenzene was filtered by the microporous filter membrane(water system) which was 0.45 μm,and then the samples diluted with methanol were injected.The qualitative analysis of the experiment was used retention qualitative method comparing directly with the known standard material,the quantitative analysis was used external standard method.The linear regression equations of nitrobenzene,aniline and p-aminophenol are obtained from experiments,and the correlation coefficients are 0.998 6,0.999 8 and 0.999 9,the detection limit is 2.0,20.0 mg/L and 21.0 mg/L,the coefficient of recoveries of them are 97.6%,97.5% and 98.1%,the precisions expressed in relative standard deviation are 0.62,0.77 and 0.36 respectively.This method is quick,accurate and simple and does not require sample pretreatment,experimental results are satisfactory comparatively.