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针对水中痕量(<1 mg/L)甲基膦酸类化合物进行了GC-MS定性分析检测研究。建立了固相萃取结合氟化物衍生的方法进行样品制备。采用600MHz核磁对氟化物衍生效率进行分析,衍生效率大于99%。采用气相色谱-电子轰击电离质谱(GC-EI/MS)、气相色谱-化学源负电离质谱(GC-NCI/MS)以及气相色谱-选择离子扫描质谱(GC-SIM-MS)分析方法对5种标准物质沙林、梭曼原体以及甲基膦酸异丙酯、甲基膦酸乙酯、甲基膦酸的衍生化产物进行了分析,检出限分别为10,50,0.2,0.1,0.05μg/L,方法的相对标准偏差小于7%。
GC-MS qualitative analysis of traces of methylphosphonates in water (<1 mg / L) was performed. A solid phase extraction coupled with fluoride derivatization was developed for sample preparation. Using 600MHz NMR analysis of fluoride derivatization efficiency, the derivatization efficiency is greater than 99%. Gas chromatography-electron impact ionization mass spectrometry (GC-EI / MS), gas chromatography-chemical negative ionization mass spectrometry (GC-NCI / MS) and gas chromatography-selective ionization mass spectrometry (GC- SIM- The species of reference material sarin, soman, as well as isopropyl methylphosphonate, ethyl methyl phosphonate, methyl phosphonic acid derivatives were analyzed, the detection limits were 10,50,0.2,0.1 , 0.05μg / L, the relative standard deviation of the method is less than 7%.