气相色谱法分析三甲基乙酰氯及其合成液的研究  

Analysis and research of trimethyl acetyl chloride and its synthetic fluid

作　　者：薛勇江 张玉亨 祝安娜 张进 

机构地区：[1]抚顺市化工研究设计院,辽宁抚顺113006

出　　处：《化学工程师》2005年第6期25-27,共3页Chemical Engineer

基　　金：国家重点科技项目(85-522-01-05);合成叔碳酸项目的下游产品曾被列为1999年抚顺市重点科技项目

摘　　要：本文利用气相色谱法对三甲基乙酰氯及其合成液进行了分析和研究。以三氯化磷为酰氯化剂,用三甲基乙酸合成三甲基乙酰氯的合成液中含有:三甲基乙酸、三氯化磷、三甲基乙酰氯、磷酸、三甲基乙酸酐、氯化氢以及其它低级脂肪酸的酰氯化物。曾试图利用填充柱进行分离定量,但因样品的性质活泼,有强烈地腐蚀性而失败;采用新方法,在样品中加入起缓冲作用的惰性物质,提高系统检测灵敏度,利用毛细管柱进行分离定量。分析条件:弹性石英毛细管柱25m×0.31mm内涂OV-1;采用分流进样技术,分流比为80:1;进样器温度150℃;检测器温度200℃;升温程序为初温70℃保持5min,升温速率20℃·min-1,终温140℃保持20min。方法中各主要产物与原料达到基线分离,难分离物质对达到峰谷分离。多次测定结果的相对误差是0.42%,相对标准偏差是0.27%。并对样品的存放条件进行了考察;对柱子的使用寿命进行了考察。Qualitative analysis/quantitative analysis of trimethyl acetyl chloride with its synthesis liquid and research , Trimethyl acetyl chloride was synthesized with trimethyl-acetyl acid and phosphorus trichloride, its synthesis liquid contain:trimethyl-acetyl acid,phosphorus trichloride,trimethyl acetyl chloride,phosphoric acid,trimethyl-acetic anhydride,hydrochloric and other impurity. A model GC112A gas chromatograph equipped with FID/TCD was used .The column is a elastic force quartz capillary tube(φ0.31mm×25m) packed with OV-1. Operating parameters: column temperature programming:70℃ (5min) then 20 ℃ ·min^(-1) to 140℃ (20min);Injecter temperature,150℃;Detector temperature 200 ℃.Analytical of composition in trimethyl acetyl chloride with its synthesis liquid be established.Each main product achieve to baseline isolation with raw material.Loath to part from each other achieve to peak valley isolation with raw aterial.The determination relative errors of quantitative calibration factor were 0.42%,and its relative standard deviation was 0.27%. Useful life of capillary tube column was in progress inspect.Storage condition of test sample was in progress inspect.

关 键 词：三甲基乙酰氯 气相色谱法分析 合成液 三甲基乙酸 石英毛细管柱 相对标准偏差 三氯化磷 低级脂肪酸 检测灵敏度 惰性物质 缓冲作用 分析条件 进样技术 升温程序 升温速率 基线分离 相对误差 测定结果 存放条件 使用寿命 

分 类 号：TQ225.22[化学工程—有机化工] TS47[农业科学—烟草工业]