Li S, Gu H, Zheng M, Zhan Y
Institute of Chemical Defence, Testing and Analysis Center, Beijing, 102205.
Se Pu. 1997 Jul;15(4):324-7.
Catalytic hydrogenation of nitrobenzene with supported palladium catalyst is a new method to produce p-aminophenol. p-Aminophenol, aniline and 4,4'-diaminodiphenyl ether obtained from this method were determined by reversed phase high performance liquid chromatography. The factors, e.g., concentration of methanol, pH and ionic strength which could affect separation efficiency were studied. UV spectra of p-aminophenol, aniline and 4,4'-diaminodiphenyl ether were recorded. Good separation was performed by using a 100 mm x 4.6 mm column with 5 microm Hypersil ODS, a mixture of 60% aqueous 8.0 mmol/L KH2PO4 buffered to 6.5 with 4.0 mmol/L Na2HPO4 and 40% methanol as mobile phase at a flow rate of 1.0 mL/min, and UV spectrophotometric detector at 232 nm wavelength. The calibration curves of p-aminophenol, aniline and 4,4'-diaminodiphenyl ether have good linearity over concentration range of 5-250, 5-150 and 0.2-120 mg/L, respectively. Minimum detectable limits at a signal-to-noise ratio of 2 were 0.1, 0.6 and 0.6 ng. This method has been applied to analysis of the reaction products of ultrasonic catalytic hydrogenation and industrial samples with good results and reproducibility.
负载型钯催化剂催化硝基苯加氢是制备对氨基苯酚的一种新方法。采用反相高效液相色谱法测定了该方法制得的对氨基苯酚、苯胺和4,4'-二氨基二苯醚。研究了甲醇浓度、pH值和离子强度等影响分离效率的因素。记录了对氨基苯酚、苯胺和4,4'-二氨基二苯醚的紫外光谱。采用100 mm×4.6 mm、5 μm的Hypersil ODS柱,以60%的8.0 mmol/L磷酸二氢钾水溶液(用4.0 mmol/L磷酸氢二钠缓冲至pH 6.5)和40%甲醇的混合溶液为流动相,流速为1.0 mL/min,在232 nm波长下用紫外分光光度检测器进行检测,实现了良好的分离。对氨基苯酚、苯胺和4,4'-二氨基二苯醚的校准曲线在5 - 250、5 - 150和0.2 - 120 mg/L的浓度范围内分别具有良好的线性关系。在信噪比为2时的最低检测限分别为0.1、0.6和0.6 ng。该方法已应用于超声催化加氢反应产物及工业样品的分析,结果良好,重现性好。