电还原邻氯硝基苯合成2,2’-二氯氢化偶氮苯电解液的高效液相色谱分析法

High Performance Liquid Chromatography Method for the Electrolyte of Electro-reduction of o-Chloronitrobenzene to 2,2’-Dichlorohydrazobenzene

实验建立了一种分析测定邻氯硝基苯电还原产物的高效液相色谱法。选用Shim-pack VP-BDS(250 mm×4.6 mm,5μm)色谱柱,245 nm为检测波长,流动相70%甲醇,流速1.2 mL/min,柱温30℃,以外标法对邻氯硝基苯、邻氯苯胺和2,2'-二氯氢化偶氮苯进行定量分析。实验结果显示,在5.0~65.0μg/mL范围内,色谱峰面积与其浓度都具有良好的线性关系,相关系数分别为r=0.9993(n=13),r=0.9993(n=13),r=0.9990(n=13),且方法的精密度良好,相对标准偏差分别为≤1.41%、≤0.65%和≤1.04%。将方法应用于以邻氯硝基苯为原料电解合成2,2'-二氯氢化偶氮苯过程中产物、副产物与剩余原料的测定,其加标回收率分别在91.3%~109.9%、90.9%~103.0%和92.3%~109.7%之间,表明方法可以同时测定邻氯硝基苯、邻氯苯胺和2,2'-二氯氢化偶氮苯的含量。

A HPLC method was established for the detection of the electroreduced o-chloronitrobenzene reaction product.The experiment was carried on a Shim-pack VP-BDS chromatographic column(250 mm×4.6 mm,5μm),the detection wavelength was 245 nm,mobile phase was 70%methanol,the flow rate was 1.2 mL/min,and the column temperature was 30℃.Quantitative analysis of o-chloronitrobenzene,o-chloraniline and 2,2'-dichlorohydrogenazobenzene was determined by external standard method.The peak area and their concentration showed a good linear relationship in the range of 5.0~65.0μg/mL,and the correlation coefficients were r=0.9993(n=13),r=0.9993(n=13),r=0.9990(n=13),and the precision of the method was good with the relative standard deviations≤1.41%,≤0.65%and≤1.04%,respectively.The method was applied to the determination of products,by-products and remaining raw materials in the process of electrolytic synthesis of 2,2'-dichlorohydrogenazobenzene with o-chloronitrobenzene as raw material.The recoveries were 91.3%~109.9%,90.9%~103.0%and 92.3%~109.7%,respectively,indicating that the method could be used for simultaneous determination of o-chloronitrobenzene,o-chloraniline and 2,2'-dichlorohydroazobenzene.