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Studies on Determination of p Aminophenol and Its Related Compounds Prepared with Catalytic Hydrogenation by Reversed Phase High Performance Liquid Chromatography

Li Shanmao, Gu Huifen, Zheng Mingsheng and Zhan Yan(Institute of Chemical Defence, Testing and Analysis Center, Beijing, 102205)  
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 100mm×4.6mm column with 5μm Hypersil ODS, a mixture of 60% aqueous 8.0mmol/L KH 2PO 4 buffered to 6.5 with 4.0mmol/L Na 2HPO 4 and 40% methanol as mobile phase at a flow rate of 1.0mL/min, and UV spectrophotometric detector at 232nm 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 120mg/L, respectively. Minimum detectable limits at a signal to noise ratio of 2 were 0.1, 0.6 and 0.6ng. This method has been applied to analysis of the reaction products of ultrasonic catalytic hydrogenation and industrial samples with good results and reproducibility.
【Fund】: 国家自然科学基金
【CateGory Index】: O658/O621
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