摘要
建立一种基于气相色谱法的精准分析方法,用于测定乙醇催化氧化合成的乙醛体系中目标产物乙醛及其潜在杂质乙醇、乙酸乙酯含量,为工艺优化与质量控制提供可靠检测手段。在选定的色谱条件,柱温100℃恒温,进样口温度220℃,检测器温度220℃,柱载气流量(高纯氮)1.0 mL/min,分流比100:1,进样量0.2μL,使用极性柱SUPELCOWAX^(TM) 10弹性石英涂渍聚乙二醇毛细管柱分离,氢火焰离子化检测器检测,采用面积归一法定量分析各组分相对含量,并验证方法的线性范围及检出限、精密度与加标回收率。乙醇催化氧化合成乙醛各组分的分离效果较好,乙醛的含量及其杂质乙酸乙酯、乙醇含量能够被准确快速地检测出,加标回收率分别为99.998%~100.066%、96.348%~105.263%、94.164%~101.235%。
A precise analysis method based on gas chromatography was established for determining the content of target product acetaldehyde and its potential impurities ethanol and ethyl acetate in the acetaldehyde system synthesized by ethanol catalytic oxidation,providing a reliable detection method for process optimization and quality control.Under the selected chromatographic conditions,the column temperature was kept at 100℃,the injection port temperature was 220℃,the detector temperature was 220℃,the column carrier gas flow rate(high-purity nitrogen)was 1.0 mL/min,the split ratio was 100:1,and the injection volume was 0.2μL.The polar column SUPERCOWAX^(TM) 10 elastic quartz coated polyethylene glycol capillary column was used for separation,and the hydrogen flame ionization detector was used for detection.The area normalization method was used to quantitatively analyze the relative content of each component,the linear range,detection limit,precision and residual recovery rate of the method were verified.The separation effect of various components in the synthesis of acetaldehyde by ethanol catalytic oxidation was good,and the content of acetaldehyde and its impurities ethyl acetate and ethanol can be accurately and quickly detected.The spiked recovery rate was from 99.998%to 100.066%,96.348%to 105.263%,and 94.164%to 101.235%,respectively.
作者
徐荣莽
罗代玉
胡田
袁红燕
XU Rongmang;LUO Daiyu;HU Tian;YUAN Hongyan(Anhui Liuliu Mei Research Institute Co.,Ltd.,Anhui Wuhu 241200;Anhui Zhongnong’an Inspection and Testing Center Co.,Ltd.,Anhui Wuhu 241200,China)
出处
《广州化工》
2025年第9期136-139,226,共5页
GuangZhou Chemical Industry
关键词
乙醇
乙酸乙酯
乙醛
气相色谱
测定
ethanol
ethyl acetate
acetaldehyde
gas chromatography
determination
