气相色谱/氢火焰离子化检测法分析烷基化物料中的C_4氟代烃  

Analysis of C_4 Fluoride Compounds in Alkylation Materials by Gas Chromatography/Flame Ionization Detection (GC/FID)

作　　者：韩江华[1] 杨海鹰[1] 

机构地区：[1]中国石油化工股份有限公司石油化工科学研究院,北京100083

出　　处：《色谱》2004年第5期504-508,共5页Chinese Journal of Chromatography

摘　　要：以实验室合成的氟代叔丁烷、氟代仲丁烷、氟代正丁烷为参考,建立了烷基化物料中C4氟代烃的气相色谱/氢火焰离子化检测(GC/FID)分析方法。提出了利用气相色谱/原子发射光谱(GC/AED)按元素响应的特点求算C4氟代烃在GC/FID上相对校正因子的方法。方法采用OV 225(50m×0 25mmi d ×0 25μm)和SE 54(44m×0 22mmi d ×0 25μm)串联柱为分析柱,FID为检测器,校正归一化或间接外标方法进行定量,具有重复性好、应用移植便利、操作简单等特点,对氟代叔丁烷的检测限为150μL/L。A method for the analysis of C_4 fluoride compounds in alkylation materials was developed by GC/FID. In order to confirm the presence of C_4 fluoride compounds in alkylation materials, 1-fluorobutane, 2-fluorobutane and 2-fluoro-2-methylpropane were synthesized and analysed by GC/FID, gas chromatography/atomic emission detection (GC/AED) and gas chromatography/mass spectrometry (GC/MS). The results showed that only 2-fluoro-2-methylpropane existed in the alkylation materials. Based on the properties of element response on GC/AED, the calibration factors of C_4 fluoride compounds on GC/FID were calculated. The analysis was performed on OV-225 (50 m×0.25 mm i.d.×0.25 μm) and SE-54 (44 m×0.22 mm i.d.×0.25 μm) columns, which were connected in series. FID was used as the detector. In quantitative analysis of the alkylation materials the methods of calibration normalization and indirect external standard were suggested. The calibration curves were linear (r=0.992) in the concentration range of 156-700 μL/L. The minimum detection limit of 2-fluoro-2-methylpropane in real samples was 150 μL/L (S/N=3). The method is simple, reproducible and easy to be applied. The other components in the alkylation materials can also be analyzed if the calibration normalization method is used.

关 键 词：气相色谱 C4氟代烃 分析 合成 

分 类 号：O658[理学—分析化学]