GC Determination of 4 Monomers in Nylon 12
摘 要
尼龙12样品(0.100 g)用六氟异丙醇1.0 mL在45℃溶解3 h。冷却后,移取上述溶液0.10 mL,加入乙酸乙酯2.0 g,密闭摇匀,静置2 h,取上层液体经过0.45 μm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×0.25 mm,0.25 μm)分离,氢火焰离子化检测器检测。4种单体的质量浓度均在2.0~200.0 mg·L-1内与其对应的峰面积呈线性关系,检出限(3S/N)为0.7~2.0 mg·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%。
Abstract
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 0.45 μm 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, 0.25 μm) 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.
中图分类号 O657.7 DOI 10.11973/lhjy-hx201905010
所属栏目 工作简报
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收稿日期 2018/8/6
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备注申学燕,高级工程师,研究方向为理化分析,xyshen@whchem.com
引用该论文: SHEN Xueyan,WANG Qingyi,ZHOU Yun,LI Jing,HUANG Changrong. GC Determination of 4 Monomers in Nylon 12[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2019, 55(5): 550~553
申学燕,王庆义,周芸,李晶,黄长荣. 气相色谱法测定尼龙12中4种单体[J]. 理化检验-化学分册, 2019, 55(5): 550~553
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【3】汪艳,史玉升,黄树槐.尼龙12热稳定性研究[J].武汉工程大学学报, 2008,30(1):59-61.
【4】李馥梅.长碳链尼龙的研究开发与应用[J].化工新型材料, 2006,34(12):6-9.
【5】王飞,王浩江,雷祖碧.玻纤增强尼龙66的抗高温热氧老化研究[J].合成材料老化与应用, 2014,43(6):7-10.
【6】王雨凝,许高燕,斯文,等.气相色谱-质谱法测定烟用辅料中的己二酸二辛酯[J].理化检验-化学分册, 2017,53(1):100-102.
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【9】陈章捷,张艳燕,钟坚海,等.气相色谱法同时测定食品模拟物中己内酰胺和十二内酰胺[J].分析试验室, 2015,34(12):1447-1450.
【10】杨先炯,王永林,王爱民,等.气相色谱法测定聚酰胺树脂中己内酰胺残留量[J].时珍国医国药, 2009,20(4):877-878.
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