蒽醌法生产过氧化氢工作液溶剂组分的气相色谱法研究  

Studies on gas chromatography of the solvent components in working solution for hydrogen peroxide production by anthraquinone process

作　　者：胡芳 刘清海 Hu Fang;Liu Qinghai(Henan Billions Advanced Material Co.,Ltd.,Jiaozuo Henan 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：《合成技术及应用》2023年第3期57-60,共4页Synthetic Technology & Application

摘　　要：根据蒽醌法生产过氧化氢中间质量控制的需求,建立了一种气相色谱法测定工作液溶剂组分的方法。采用TG-5SILMS(30 m×0.25 mm,0.25μm)毛细管柱,程序升温,起始温度40℃,保持3 min,以10℃/min升到300℃并保持1 min,进样口温度300℃,分流进样,分流比为100∶1,氢火焰离子化(FID)检测器,检测器温度300℃,进样量1.0μL的检测条件,先根据重芳烃(AR)、四丁基脲(TBU)和磷酸三辛酯(TOP)单标的保留时间进行定性分析,再采用一点校正法对工作液各溶剂组分进行定量分析。结果表明:该方法操作简单、相对标准偏差在0.18%~0.38%之间、加标回收率在99.85%~100.68%之间,可作为蒽醌法生产过氧化氢中间过程质量控制。A method for the determination of the solvent components in working solution by gas chromatography has been developed on the background of intermediate quality control in the production process of hydrogen peroxide by anthraquinone process.The analytical condition was based on TG-5SILMS(30 m×0.25 mm,0.25μm)capillary column with programmed temperature steps,the initial column temperature was 40℃,maintained 3 min,then rised to 300℃with the speed of 10℃/min,maintained 1 min.The inlet temperature was 300℃with the split ratio 100∶1.The detector was FID with temperature of 300℃and the injection volume was 1.0μL.First,the retention time of Heavy aromatics(AR),Tetrabutylurea(TBU),Tris(2-ethylhexyl)phosphate(TOP)was analyzed qualitatively,and then the one point correction method was applied to the quantitative analysis of the solvent components in working solution.The results showed that the relative standard deviation about the components of working solution and recovery rate were 0.18%~0.38%and 99.85%~100.68%seperatively by this simple method.

关 键 词：气相色谱法 氢火焰离子化检测器 保留时间 定量分析 重芳烃 四丁基脲 磷酸三辛酯 

分 类 号：O657[理学—分析化学]