An Approach for Simultaneous Determination of Cyclohexanone Oxime and Hydroxylammonium Sulfate in the Hydrolysis of Cyclohexanone Oxime

doi:10.11944/j.issn.1000-0518.2015.11.150138

Chinese Journal of Applied Chemistry ›› 2015, Vol. 32 ›› Issue (11): 1312-1318.DOI: 10.11944/j.issn.1000-0518.2015.11.150138

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An Approach for Simultaneous Determination of Cyclohexanone Oxime and Hydroxylammonium Sulfate in the Hydrolysis of Cyclohexanone Oxime

ZHAO Fangfang^a,YOU Kuiyi^a^b^*(),PENG Chao^a,TAN Shan^a,LIU Pingle^a^b,WU Jian^a^b,LUO Hean^a^b

^aSchool of Chemical Engineering
^bNational & Local United Engineering Research Center for Chemical Process Simulation and Intensification, Xiangtan University,Xiangtan,Hu'nan 411105,China

Received:2015-04-14 Accepted:2015-06-26 Published:2015-11-02 Online:2015-11-02
Contact: YOU Kuiyi
Supported by:
Supported by the National Natural Science Foundation of China(No.21276216), Scientific Research Fund of Hunan Provincial Education(No.13A096)

Abstract

Abstract:

Hydroxylammonium sulfate(HAS) and cyclohexanone oxime(CHO) are difficult to be separated in acidic media in the hydrolysis of CHO. Thus, it is difficult to determinate HAS accurately by redox titration method due to the interference of CHO. A simple and efficient approach for simultaneous determination of HAS and CHO in the hydrolysis reaction of CHO was successfully developed by combining redox titration and high performance liquid chromatography in this article. With the concentration of H⁺ over 2.4 mol/L and the molar ratio of Fe³⁺ to CHO over 5:1, the relative standard deviation are 0.39% and 0.50%, and the correlation coefficients are 0.99998 and 0.99996 for five determinations of CHO and HAS, respectively. The recoveries of test samples are between 97.1% and 100.6%.

Key words: hydrolysis reaction, cyclohexanone oxime, hydroxylamine sulfate, high performance liquid chromatography, redox titration

ZHAO Fangfang, YOU Kuiyi, PENG Chao, TAN Shan, LIU Pingle, WU Jian, LUO Hean. An Approach for Simultaneous Determination of Cyclohexanone Oxime and Hydroxylammonium Sulfate in the Hydrolysis of Cyclohexanone Oxime[J]. Chinese Journal of Applied Chemistry, 2015, 32(11): 1312-1318.

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An Approach for Simultaneous Determination of Cyclohexanone Oxime and Hydroxylammonium Sulfate in the Hydrolysis of Cyclohexanone Oxime

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