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Citation: 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. doi: 10.11944/j.issn.1000-0518.2015.11.150138 shu

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

1.
a School of Chemical Engineering, Xiangtan University, Xiangtan, Hu'nan 411105, China;
2.
b National & Local United Engineering Research Center for Chemical Process Simulation and Intensification, Xiangtan University, Xiangtan, Hu'nan 411105, China

Corresponding author: YOU Kuiyi,
Received Date: 14 April 2015
Available Online: 26 May 2015
Fund Project: 国家自然科学基金(21276216) (21276216)湖南省教育厅重点项目(13A096)资助 (13A096)

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%.
- hydrolysis reaction,
- cyclohexanone oxime,
- hydroxylamine sulfate,
- high performance liquid chromatography,
- redox titration
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