首页|定量核磁共振波谱法快速测定灭火剂材料中全氟辛烷磺酰基化合物

定量核磁共振波谱法快速测定灭火剂材料中全氟辛烷磺酰基化合物

Rapid Determination of Perfluoroalkyl Sulfonyl Compounds in Foam Extinguishing Agents by Nuclear Magnetic Resonance Spectroscopy

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泡沫灭火剂中全氟辛烷磺酰基化合物(PFOS)的使用受到严格管控.针对灭火剂中PFOS快速测定的需求,建立了基于19F的定量核磁共振波谱(qNMR)检测方法.方法以全氟丁基磺酸钾为标准物质,通过计算全氟丁基磺酸钾的-CF3 在化学位移δ-78.94处19F特征峰和PFOS的-CF2 在化学位移δ-117.12处19F特征峰的积分面积比值,进而实现PFOS定量分析.经测试,全氟丁基磺酸钾百分含量与定量峰面积线性相关系数为 0.995 5,检出限为0.024％,定量限为 0.080％.8种灭火剂产品的定性测定结果与实际标注情况相吻合,其中 4种泡沫灭火剂产品中PFOS含量在 0.106％～1.339％之间.研究结果表明,方法受基质干扰小、检测速度快、灵敏度高,可为泡沫灭火剂中PFOS的管控提供可靠的检测方法与数据支撑.
The usage of perfluorooctane sulfonyl compounds(PFOS)in foam extinguishing agents is strictly regulated.A quantitative nuclear magnetic resonance spectroscopy(qNMR)detection method based on 19F was established for the rapid determination of PFOS in fire extinguishing agents.Using potassium perfluorobutylsulfonate as the standard substance,the quantitative analysis of PFOS could be realized by calculating the integral area ratio of the 19F characteristic peak of-CF3 in potassium perfluorobutylsulfonate at chemical shift δ-78.94 and the 19F characteristic peak of-CF2 in PFOS at chemical shift δ-117.12.The linear correlation coefficient between the percentage content of potassium perfluorobutylsulfonate and the quantitative peak area was 0.995 5,the limit of detection was 0.024％,and the limit of quantitative was 0.080％.The qualitative determination results of 8 foam extinguishing agent products were consistent with the actual labeling,and the content of PFOS in 4 foam extinguishing agent products was 0.106％～1.339％.The research results showed that the method has the advantages of low matrix interference,fast detection speed,and high sensitivity,which could provide a reliable detection method and data support for the regulation of PFOS in foam extinguishing agents.

perfluorooctane sulfonyl compoundsfoam extinguishing agentquantitative nuclear magnetic resonance spectroscopypotassium perfluorobutylsulfonate

李杨、黄卫、王畅、李洋、花磊、田颖

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中国科学院大连化学物理研究所,辽宁 大连 116023

大连交通大学,辽宁 大连 116023

吉林工商学院,吉林 长春 130507

全氟辛烷磺酰基化合物 泡沫灭火剂 定量核磁共振波谱法 全氟丁基磺酸钾

国家自然科学基金项目大连化物所创新研究基金项目辽宁省中央引导地方科技发展资金

22174142DICP I2021442023JH6/100100057

2024

10.16495/j.1006-3757.2024.01.006

分析测试技术与仪器
中国科学院兰州化学物理研究所,中国科学院计划财务局,中国科学院兰州分院分析测试中心

分析测试技术与仪器

影响因子：0.444
ISSN：1006-3757
年,卷(期)：2024.30(1)
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