顶空气相色谱法测定苯酚丙酮装置废水中甲基过氧化氢含量  

Determination of methyl hydrogen peroxide in wastewater from phenol-acetone plant by headspace gas chromatography

作　　者：董鑫 蔡登定 赵泳立 王欣 DONG Xin;CAI Deng-ding;ZHAO Yong-li;WANG Xin(Inspection Center of Zhejiang Petroleum&Chemical Co Ltd,Zhoushan 316000,China)

机构地区：[1]浙江石油化工有限公司化验中心,浙江舟山316000

出　　处：《石化技术与应用》2024年第4期302-305,共4页Petrochemical Technology & Application

基　　金：浙江石油化工有限公司科技开发项目(项目编号:ZSH-RD-23-101)。

摘　　要：建立了一种采用顶空气相色谱法快速测定苯酚丙酮装置废水中过氧化物的方法,其中主要过氧化物甲基过氧化氢,通过衍生化反应后测定,对该方法的准确度、精密度、重复性进行了分析。结果表明:以醋酸作为衍生化反应的酸性试剂,碘化钾水溶液质量分数为50%时,甲基过氧化氢衍生化反应最完全;在顶空平衡温度为80℃,顶空平衡时间为12 min时,样品含甲醇量的测定值与实际值最为接近;该方法具有较高的准确度和重复性,相对标准偏差为0.027%。A method for rapid determination of peroxides in wastewater from phenol-acetone plant by headspace gas chromatography was established.The main peroxide,methyl hydrogen peroxide was determined by derivatization reaction.The accuracy,precision and repeatability of this method were analyzed.The results showed that the derivatization of methyl hydrogen peroxide was the most complete when the mass fraction of potassium iodide solution was 50%with acetic acid as the acid reagent.When the headspace equilibrium temperature was 80℃and the headspace equilibrium time was 12 min,the measured methanol content of the sample was the closest to the actual value.The method had high accuracy and repeatability,and the relative standard deviation was 0.027%.

关 键 词：顶空气相色谱法 甲基过氧化氢 醋酸 碘化钾 甲醇 衍生 

分 类 号：TQ019[化学工程]