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

应用化学, 2015, 32(11): 1312-1318. doi: 10.11944/j.issn.1000-0518.2015.11.150138

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

赵方方 ^1, , 游奎一 ^2, , 彭超 ^3, , 谭珊 ^4, , 刘平乐 ^5, , 吴剑 ^6, , 罗和安 ^7,

1.湘潭大学化工学院湖南湘潭411105

2.湘潭大学化工学院湖南湘潭411105;湘潭大学化工过程模拟与强化国家地方联合工程研究中心湖南湘潭411105

3.湘潭大学化工学院湖南湘潭411105

4.湘潭大学化工学院湖南湘潭411105

5.湘潭大学化工学院湖南湘潭411105;湘潭大学化工过程模拟与强化国家地方联合工程研究中心湖南湘潭411105

6.湘潭大学化工学院湖南湘潭411105;湘潭大学化工过程模拟与强化国家地方联合工程研究中心湖南湘潭411105

7.湘潭大学化工学院湖南湘潭411105;湘潭大学化工过程模拟与强化国家地方联合工程研究中心湖南湘潭411105

基金项目: 湖南省教育厅重点项目(13A096) the National Natural Science Foundation of China(21276216) 国家自然科学基金(21276216) Scientific Research Fund of Hunan Provincial Education(13A096)

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

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

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

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％.

参考文献

[1]	高丽雅;檀学军;张东升;王淑芳;赵新强;王延吉.羟胺（盐）的合成及其应用研究进展[J].化工进展,2012(9):2043-2048.
[2]	Raman S;Ashcraft RW;Vial M;Klasky ML.Oxidation of hydroxylamine by nitrous and nitric acids. Model development from first principle SCRF calculations[J].The journal of physical chemistry, A. Molecules, spectroscopy, kinetics, environment, & general theory,200538(38):8526-8536.
[3]	Yi-Ping Chang;Kenneth K. Kuo.Assessment of Combustion Characteristics and Mechanism of Hydroxylammonium Nitrate-Based Liquid Monopropellant[J].Journal of Propulsion & Power,20025(5):1076-1085.
[4]	Zhao, Fangfang;You, Kuiyi;Li, Ruige;Tan, Shan;Liu, Pingle;Wu, Jian;Ai, Qiuhong;Luo, He'an.Novel Approach for the Preparation of Hydroxylammonium Nitrate from the Acid-Catalyzed Hydrolysis of Cyclohexanone Oxime[J].Industrial & Engineering Chemistry Research,20153(3):819-823.
[5]	Zhao, Fangfang;You, Kuiyi;Peng, Chao;Tan, Shan;Li, Ruige;Liu, Pingle;Wu, Jian;Luo, He'an.A simple and efficient approach for preparation of hydroxylamine sulfate from the acid-catalyzed hydrolysis reaction of cyclohexanone oxime[J].Chemical engineering journal,2015:102-107.
[6]	Tawan Sooknoi;Veerachai Chitranuwatkul.Ammoximation of cyclohexanone in acetic acid using titanium silicalite-1 catalyst:Activity and reaction pathway[J].Journal of molecular catalysis, A. Chemical,20051/2(1/2):220-226.
[7]	J. S. Zhang;K. Wang;Y. C. Lu.Beckmann Rearrangement of Cyclohexanone Oxime in a Microchemical System: The Role of SO3 and Product Inhibition[J].AIChE Journal,201210(10):3156-3160.
[8]	Guzowski JP;Golanoski C;Montgomery ER.A gas chromatographic method for the indirect determination of hydroxylamine in pharmaceutical preparations: conversion into nitrous oxide.[J].Journal of Pharmaceutical and Biomedical Analysis: An International Journal on All Drug-Related Topics in Pharmaceutical, Biomedical and Clinical Analysis,20035(5):963-974.
[9]	Zhang, H.;Zheng, J..Sensitive detection of hydroxylamine at a simple baicalin carbon nanotubes modified electrode[J].Talanta: The International Journal of Pure and Applied Analytical Chemistry,2012:67-71.

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