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Rapid determination of products of phenol hydrogenation in a supercritical water system using headspace gas chromatography

Qing-Qing Guan, Xiao-Dian Huang, Yan-Hua Zeng, Chao-Hai Wei, Ping Ning, Jun-Jie Gu, and Xin-Sheng Chai

Faculty of Environmental Science and Engineering, Kunming University of Science and Technology, 727 South Jingming Rd, Kunming 650500, China



Abstract: This paper reports a headspace analysis technique for the determination of products, i.e., cyclohexanone (CE) and cyclohexanol (CL), of phenol hydrogenation in a supercritical water reaction system (SWRS) with water removal by hydrate formation. An addition of anhydrous calcium chloride leads to water absorption resulting in crystal water; thus, the samples can be quantitatively measured without the influence of water. After achieving equilibrium at 150­°C and maintaining it for 5 min, the obtained results showed a relative standard deviation of less than 5.3 % and the recovery ranged from 93 % to 104 %. The presented method is simple and accurate for the analysis of CL, CE and phenol in samples from phenol conversion in SWRS.

Keywords: headspace analysis – water removal by hydrate formation – hydrogenation of phenol – supercritical water

Full paper is available at

DOI: 10.1515/chempap-2015-0081


Chemical Papers 69 (5) 662–667 (2015)

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