气相色谱法测定尼龙12中4种单体

尼龙12样品(0.100g)用六氟异丙醇1.0mL在45℃溶解3h。冷却后,移取上述溶液0.10mL,加入乙酸乙酯2.0g,密闭摇匀,静置2h,取上层液体经过0.45μm亲水聚四氟乙烯针式过滤器。采用气相色谱法测定滤液中4种单体的含量。4种单体用RXI^-17色谱柱(30 m×0.25mm,0.25μm)分离,氢火焰离子化检测器检测。4种单体的质量浓度均在2.0～200.0mg·L^-1内与其对应的峰面积呈线性关系,检出限(3S/N)为0.7～2.0mg·L^-1。方法用于尼龙12样品的分析,加标回收率为93.7%～115%,测定值的相对标准偏差(n=6)为1.5%～3.2%。

GC Determination of 4 Monomers in Nylon 12

The nylon 12 sample(0.100 g) was dissolved for 3 h with 1.0 mL of hexafluoroisopropanol at 45℃.After cooling,0.10 mL of the above solution was taken and 2.0 g of ethyl acetate was added.After shaking up in airtight container,the mixed solution was stood for 2 h.The supernatant liquid was filtered on 0.45μm needle filter of hydrophilic PTFE.GC was applied to the determination of 4 monomers in the filtrate.The 4 monomers were separated on RXI-17 chromatographic column(30 m×0.25 mm,0.25μm) and detected by FID.Linear relationships between values of peak area and mass concentration of the 4 monomers were kept in the same range of 2.0-200.0 mg·L-1,with detection limits(3S/N) in the range of 0.7-2.0 mg·L-1.The proposed method was applied to the analysis of the nylon 12 sample,giving values of recovery found by standard addition method and RSDs(n=6) of determined values in the ranges of 93.7%-115% and 1.5%-3.2% respectively.