一种同时测定环己酮肟水解反应中环己酮肟和硫酸羟胺含量的方法

doi:10.11944/j.issn.1000-0518.2015.11.150138

摘要/Abstract

摘要：

在环己酮肟水解反应制备硫酸羟胺过程中,环己酮肟与产物硫酸羟胺在酸性条件下难以分离,硫酸羟胺的含量测定受到环己酮肟的干扰。本文采用高效液相色谱法和氧化还原滴定法建立了一种简便、有效的新方法同时测定硫酸羟胺与环己酮肟的含量。结果表明,在H⁺浓度大于2.4 mol/L,Fe³⁺/环己酮肟摩尔比大于5:1的条件下,环己酮肟和硫酸羟胺测定的标准滴定曲线的线性相关系数分别为0.99998和0.99996,相对标准偏差分别为0.39%和0.50%,水解反应样品的加标回收率为97.1%~100.6%。

关键词: 水解反应, 环己酮肟, 硫酸羟胺, 高效液相色谱法, 氧化还原滴定法

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

赵方方, 游奎一, 彭超, 谭珊, 刘平乐, 吴剑, 罗和安. 一种同时测定环己酮肟水解反应中环己酮肟和硫酸羟胺含量的方法[J]. 应用化学, 2015, 32(11): 1312-1318.

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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