气相-液相色谱法分析蒽醌法双氧水工作液的组成  

Composition for hydrogen peroxide working solution in anthraquinone process using GC‑HPLC method

作　　者：胡芳 HU Fang(Henan Billions Advanced Material Co.,Ltd.,Jiaozuo 454191,China)

机构地区：[1]河南佰利联新材料有限公司,河南焦作454191

出　　处：《精细石油化工进展》2023年第5期53-58,共6页Advances in Fine Petrochemicals

摘　　要：根据蒽醌法生产双氧水的中间质量控制的需求,建立了一种气相色谱法(GC)、液相色谱法(HPLC)共同测定工作液组成的方法。结果表明:气相色谱法、液相色谱法可分别准确测定蒽醌法生产双氧水工作液中3种溶剂的体积分数、2种有效蒽醌的质量浓度,AR、TBU和TOP的保留时间依次为7.205~10.211(最高峰7.955)、18.645和24.292 min,而EAQ和THEAQ的保留时间分别为8.275和11.080 min。经检测,2022年10月14日某公司某批次的工作液中AR、TBU和TOP的体积分数依次为76.85%、3.97%和17.73%,EAQ、THEAQ分别为117.41和29.77 g/L,有效蒽醌相对标准偏差(RSD)为0.08%~1.55%、加标回收率为98.97%~100.91%。该法可为蒽醌法生产双氧水的中间过程提供质量控制。A method for the determination of the working solution compositions by gas chromatography(GC)and high performance liquid chromatography(HPLC)has been developed to take central control for analysis in the production process of hydrogen peroxide by anthraquinone process.Results showed that the volume ratio of three kinds of solvents and the mass concentration of two kinds of effective anthraquinones in working solu⁃tion for hydrogen peroxide production by anthraquinone process could be accurately determined by GC and HPLC,such as the retention time of AR,TBU and TOP was 7.205~10.211(highest peak of 7.955),18.645 and 24.292 min,as well as the retention time of EAQ and THEAQ was 8.275 and 11.080 min respectively.Af⁃ter testing,the volume fraction of AR,TBU and TOP was 76.85%,3.97%and 17.73%,and the mass concen⁃tration of EAQ and THEAQ was 117.41 and 29.77 g/L in the circulated working solution sample on October 14,2022 from some company respectively,which could be used for monitoring the intermediate process quali⁃ty of hydrogen peroxide production by anthraquinone process.The relative standard deviation(RSD)the effec⁃tive anthraquinones in working solution and recovery rate were 0.08%-1.55%and 98.97%-100.91%rsepec⁃tively.

关 键 词：气相色谱法 高效液相色谱法 双氧水工作液 蒽醌法 2-乙基蒽醌 2-乙基四氢蒽醌 

分 类 号：TQ123.6[化学工程—无机化工] O657.7[理学—分析化学]