摘要
芳纶纤维在合成过程中常使用N-甲基吡咯烷酮作为反应溶剂,通过对提取方法和色谱、质谱条件的改进,建立了芳纶纤维中溶剂残留物N-甲基吡咯烷酮（NMP）的气相色谱-质谱联用（GC/MS）测定法.芳纶纤维试样经乙酸乙酯超声波提取,提取液浓缩后用滤纸过滤,用气相色谱-质谱仪测定,外标法定量,选择离子监测进行阳性确证.结果表明,当添加N-甲基吡咯烷酮1~10μg/mL时,待测芳纶纤维试样中N-甲基吡咯烷酮的回收率达95.8%,相对标准偏差RSD（n=7）小于5%,其最低检出限为0.05μg/mL.本方法操作简单、灵敏度高、重现性好,可用于芳纶纤维中N-甲基吡咯烷酮残留量分析.
N-methylpyrrolidinone （NMP） was commonly used as reaction solvents in the synthesis of ara-mid fiber. A gas chromatography/mass spectrometry （GC/MS） method of determination of N-methylpyrrolidi-none in textiles was established by improving the extraction method and GC/MS conditions. The samples were extracted with ethyl acetate by ultrasound assisted procedure.After being concentrated and purified with filter paper, the extract was quantitatively determined using GC/MS by external standard method and positive-ly confirmed through selected-ion monitoring mode. The results showed that while the dosage of N-methyl-pyrrolidinone was 1~10 μg/mL, the method provided 95.8% of recovery rate, lower than 5% of relative stan-dard deviations and 0.05 μg/mL of determination limit. The method was simple, and had high sensitivity and good repeatability, which could be used in the residual content determination of NMP in aramid fiber.
出处
《印染助剂》
CAS
北大核心
2014年第8期50-52,共3页
Textile Auxiliaries
基金
广东省科技计划项目(2011B010400019)
广东省科技计划项目(2011GDK26)
