摘要
建立了超声提取-全蒸发顶空-气相色谱法同时测定纺织品中N，N-二甲基甲酰胺（DMF）、N，N-二甲基乙酰胺（DMAC）、N-甲基吡咯烷酮（NMP）、甲酰胺（FMA）四种溶剂残留的方法。样品经丙酮超声提取后，取微量提取液在150℃下加热20min，使其完全蒸发，抽取顶空气体进气相色谱，用氢火焰离子化检测器（FID）检测。以保留时间定性，内标法定量，以N，N-二甲基丙酰胺（DMP）作内标物。结果表明，DMF、DMAC、NMP在0．8，100μg范围内，FMA在2～100μg范围内，线性关系良好；四种物质的平均回收率为82．5％～96．1％；RSD（n=6）为1．6％。2．8％；DMF、DMAC、NMP方法检出限均为30μg／g，FMA方法检出限为80μg／g。本法操作简单、准确性高、重复性好，可用于纺织品中DMF、DMAC、NMP、FMA残留量的分析。
A method is developed for simultaneous determination of residual solvents of DMF, DMAC, NMP and FMA in textiles by ultrasonic extraction-full evaporation headspace-gas chromatography. After the samples are extracted by acetone, a small quantity of extracted solution is moved into headspace vi- al, heated at 150 ℃ for 20 rain and fully evaporated. Then the headspace gas is extracted and injected in- to gas chromatograph for analysis through flame ionization detector （FID）. Internal standard method is used for quantization with DMP as the internal standard, and retention time is used for qualitative analy- sis. The results show a good linear relationship in the ranges from 0.8 μg to 100 μg for DMF, DMAC, NMP, and from 2 μg to 100 μg for FMA. The average recovery rates of DMF, DMAC, NMP and FMA are 82.5%-96.1%, relative standard deviation （RSDs） （n=6）are !.6%-2.8% and the lowest detection limits are 30 μg/g for DMF, DMAC, NMP and 80 μg/g for FMA. This method has many advantages as follows： sim- plicity, high accuracy and good repeatability, which is suitable for the rapid analysis of residual DMF, DMAC, NMP and FMA in textiles.
出处
《印染》
北大核心
2016年第15期47-50,共4页
China Dyeing and Finishing
基金
上海检验检疫局科研项目(HK017-2014)
关键词
测试
超声提取
全蒸发顶空
气相色谱法
纺织品
有机溶剂
testing
ultrasonic extraction
full evaporation headspace
gas chromatography
textiles
organic solvents
