反相高效液相色谱法测定对硝基氯苯、对氯苯胺和苯胺  

SIMULTANEOUS DETERMINATION OF p-CHLORONITROBENZENE,p-CHLOROANILINE AND ANILINE BY REVERSED-PHASE HIGH PERFORMANCE LIQUID CHROMATOGRAPHY

作　　者：李秀瑜[1] 侯都兴[2] 赵爱东[1] 

机构地区：[1]河北师范大学实验中心,河北石家庄050016 [2]国家体育用品质量监督检验中心,河北石家庄050051

出　　处：《精细石油化工》2008年第4期52-55,共4页Speciality Petrochemicals

基　　金：河北省教育厅科研项目基金资助(990220)

摘　　要：建立了一种同时测定对硝基氯苯、对氯苯胺和苯胺含量的反相高效液相色谱法(HPLC)。HPLC 条件为:C18色谱柱,流动相 V(甲醇):V(水)=75:25,流速1 mL/min,检测波长295 nm,对硝基氯苯的加样回收率101.5%～103.7%,相对标准偏差0.605%～0.782%(n=5);对氯苯胺的加样回收率94.58%～97.35%,相对标准偏差0.605%～0.782%;苯胺加样回收率102.1%～105.8%,相对标准偏差2.04%～2.16%。该法具有较好的精密度和回收率,所得回归方程线性范围宽,适用范围广。A new reversed-phase high performance liquid chromatographic （RP-HPLC） method was developed for the simultaneous determination of p-chloronitrobenzene （p-CNB）, p-chloroaniline （p-CAN） and aniline（AN） which are the raw materials, product and dechloro-byproduct in the process of liquid phase selective hydrogenation of p-chloronitrobenzene（p-CNB） to p-chloroaniline（p- CAN）. A Ultimate C18 column was used with a mixture of methanol ： water = 75 ： 25 （volume） as the mobile phase at a flow rate of 1.0 mL/min and with a UV detector at 295 nm. The linear ranges of p-CNB, p-CAN and AN were 0. 000 498 - 1 060, 0. 005 029 - 1 070 and 0. 004 837 - 1 029 mg/L, respectively. Recoveries of p-CNB were 101.5%-103.7% with relative standard deviations（RSDs） from 0. 605% to 0. 782% （n= 5）. Recoveries of p-CAN were 94. 58%- 97. 35% with RSDs from 1.07% to 1.41%（n=5）. Recoveries of AN were 102.1%- 105.8% with the RSDs from 2.04% to 2.16%（n=5）. This method is simple, rapid and accurate which is useful for optimizing the reaction conditions and controlling the production process as well as determining the contents of the titled chemicals in waste liquids.

关 键 词：反相高效液相色谱法 对硝基氯苯 对氯苯胺 苯胺 

分 类 号：O657.71[理学—分析化学]