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建立了鞋材中丙烯腈单体残留量测定的顶空气相色谱方法。样品经N,N-二甲基甲酰胺萃取后,在极性柱上进行分离,选用氢离子火焰检测器检测,外标法定量分析。丙烯腈在50~1000mg/kg样品含量范围内线性良好,检出限为15mg/kg。选用常用鞋材锦纶、腈纶、鞋用胶粘剂、ABS橡胶、丁腈橡胶,在4个浓度水平进行添加试验,样品加标回收率在85.6%~109.5%,相对标准偏差1.98%~3.98%(n=7)。本方法操作简单快速,重现性好,准确度高。
A headspace gas chromatographic method for the determination of residual acrylonitrile monomer in shoe materials was established. Samples were extracted with N, N-dimethylformamide, and then separated on a polar column. The samples were detected by hydrogen ion flame detector and quantified by external standard method. Acrylonitrile linear in the range of 50 ~ 1000mg / kg sample content, the detection limit of 15mg / kg. The common shoe materials such as nylon, acrylic, shoe adhesive, ABS rubber and nitrile butadiene rubber were added in four levels. The recoveries were 85.6% -109.5% and the relative standard deviations were 1.98% ~ 3.98% (n = 7). The method is simple, rapid, reproducible, and highly accurate.