摘要
建立定量核磁共振氢谱法测定聚醚中醛含量。以对苯二甲酸二甲酯为内标,脉冲序列为zg30,延迟时间为10 s,采样次数为128次。以对苯二甲酸二甲酯中化学位移δ 8.10×10-6的峰为内标定量峰,根据积分面积比与质量比对醛含量进行定量分析(醛含量以乙醛计)。定量氢谱中,乙醛与内标对苯二甲酸二甲酯的质量比在0.13~1.96内与乙醛与对苯二甲酸二甲酯的定量峰积分面积比值线性关系良好,线性回归方程为y=0.469 7x+0.023 7,相关系数为0.999 6,定量限为4.33 mg/kg,精密度试验测定结果的相对标准偏差为1.8%(n=6),样品加标回收率为100.6%~104.7%。qHNMR法测定含量结果与液相色谱法测定含量结果基本一致。该方法无须样品衍生化处理,简便快捷,可为工业检测聚醚中醛含量提供一种快速有效的方法。
A quantitative proton nuclear magnetic resonance(qHNMR)method for the determination of the contents of aldehydes in polyethers was established.Dimethyl terephthalate was used as the internal standard,the pulse sequence was zg30,the delay time was 10 s,and the sampling times were 128 times.The peak of chemical shiftδ8.10×10-6 in dimethyl terephthalate was used as the internal standard quantitative peak,and the aldehyde content was quantitatively analyzed according to the integral area ratio and mass ratio(aldehyde content was calculated by acetaldehyde).In the quantitative hydrogen spectrum,the mass ratio of acetaldehyde to the internal standard dimethyl terephthalate was within 0.13-1.96 and the quantitative peak integral area ratio of acetaldehyde to dimethyl terephthalate had a good linear relationship.The regression equation was y=0.4697x+0.0237,the correlation coefficient was 0.9996.The quantification limit was 4.33 mg/kg,and the relative standard deviation of precision test results was 1.8%(n=6).The recoveries of spiked samples were in the range of 100.6%-104.7%.The contents of aldehydes by qHNMR was basically consistent with those determined by liquid chromatography.This method is simple and rapid without sample derivatization,which can provide a rapid and effective method for industrial determination of aldehydes content in polyether.
作者
丁宇
赵静文
唐福伟
叶达峰
孟佳磊
莫琴亮
DING Yu;ZHAO Jingwen;TANG Fuwei;YE Dafeng;MENG Jialei;MO Qinliang(Zhejiang Green Branch Chemical Co.,LTD.,Shaoxing 312369,China)
出处
《化学分析计量》
2025年第2期94-98,共5页
Chemical Analysis And Meterage
关键词
定量核磁共振氢谱法
聚醚
醛
对苯二甲酸二甲酯
quantitative proton magnetic resonance
polyether
aldehydes
dimethyl terephthalate
