顶空-气相色谱法快速测定三聚氰胺甲醛树脂中残留微量三乙胺  

Rapid determination of residual triethylamine in melamine formaldehyde resin by headspace-GC

作　　者：黄飞 卢科 赵婷 俞英珍 许义 范斌 HUANG Fei;LU Ke;ZHAO Ting;YU Yingzhen;XU Yi;FAN Bin(Hangzhou Transfar Fine Chemical Co.,Ltd.,Hangzhou 311215,China)

机构地区：[1]杭州传化精细化工有限公司,浙江杭州311215

出　　处：《印染》2021年第11期62-66,共5页China Dyeing and Finishing

摘　　要：建立了一种快速检测三聚氰胺-甲醛树脂中微量三乙胺的顶空-气相分析方法,并进行验证。方法采用外标法进行定量,以体积比为10∶1的11%氢氧化钠-异丙醇混合溶液作为溶剂,采用顶空-气相色谱法进行检测。色谱条件为:色谱柱选择DB-624毛细管柱(30 m×0.53 mm×3.0μm);柱温采取程序升温模式:初始柱温为100℃,保持5 min,再以25℃/min的升温速率升至240℃,保持15 min,分流比为40∶1;进样口温度为280℃,检测器温度为280℃,载气为氮气,恒定线速度为40 cm/s,进样体积为1.0 mL,80℃顶空平衡30 min。结果表明,三乙胺在选定条件下能实现很好的色谱分离,在0.254~5.080 mg/L范围内线性关系良好,R^(2)=0.9999,仪器检出限(3倍信噪比)为0.04458 mg/L,定量限(10倍信噪比)为0.1486 mg/L,相对标准偏差(RSD,n=5)小于2.2%,平均加标回收率为89.1%~110.0%。A headspace-gas phase analysis method for rapid detection of triethylamine in melamine-formalde⁃hyde resin is established and verified.The method uses an external standard method for quantification,uses 11%sodium hydroxide-isopropanol mixed solution with a volume ratio of 10∶1 as the solvent,and uses headspace-gas chromatography for detection.The chromatographic conditions are:DB-624 capillary column(30 m×0.53 mm×3.0μm)is selected for the chromatographic column;the column temperature is programmed:the initial column temperature is 100℃,keep it for 5 minutes,and then rise to 240℃at the heating rate of 25℃/min for 15 min,split ratio is 40∶1;injection port temperature is 280℃,detector temperature is 280℃,carrier gas is nitrogen,constant linear velocity is 40 cm/s,injection volume is 1.0 mL,headspace equilibration at 80℃for 30 min.The results show that triethylamine can achieve good chromatographic separation under the selected conditions,and the linear relationship is good in the range of 0.254-5.080 mg/L,R^(2)=0.9999 and the detection limit of the instrument(3 times the signal-to-noise ratio)is 0.04458 mg/L,the limit of quantification(10 times the signal-to-noise ratio)is 0.1486 mg/L,the relative standard deviation(RSD,n=5)is less than 2.2%,and the average recovery rate is 89.1%-110.0%.

关 键 词：测试 顶空-气相色谱 三聚氰胺-甲醛树脂 三乙胺 挥发性有机化合物 

分 类 号：TS197[轻工技术与工程—纺织化学与染整工程]