知识与财富的链接
实验室研制了低能光电子磁场增强电离(MEPEI)和单光子电离(SPI)复合电离源,该电离源具有电离化合物范围宽、碎片离子少、质谱图简单等优点,结合飞行时间质谱(TOF-MS)实现了聚氯乙烯(PVC)热分解/燃烧产物的在线分析.针对不同的目标化合物,MEPEI/SPI复合电离源通过调节电离区电场强度,可以快速在SPI和SPI-MEPEI之间切换.PVC热分解/燃烧产物中电离能大于光子能量(10.60 eV)的HCl和CO2(12.74 eV、13.77 eV)利用MEPEI模式电离;而烯烃、二氯乙烯、苯系物、氯苯、苯乙烯、茚满及萘系物等可通过SPI-MEPEI复合模式电离.通过实时监测PVC主要燃烧产物的信号强度随温度的变化趋势可推断出,PVC燃烧产物主要是通过两种机制生成:①250～370℃时,PVC发生脱氯及分子内环化反应,产生大量的HCl、苯和萘;②380～510℃时,PVC发生分子间交联反应,生成烷基芳烃,如甲苯和二甲苯/乙苯等.实验结果表明,SPI/SPI-MEPEI复合离子源TOF-MS分析速度快,应用范围广,在在线分析中具有广泛的应用前景.
With the features of a broad range of ionizable compounds, reduced fragments and simple mass spectrum, a homemade magnetic field enhanced photoelectron ionization (MEPEI) source combined with single photon ionization (SPI) for time-of-flight mass spectrometer was built and applied to analyze thermal decomposition/combustion products of polyvinyl chloride (PVC). The combined ion source can be switched very fast between SPI mode and SPI-MEPEI mode for detecting different targeted compounds, and only adjusting the voltage of the electrode in the ionization region to trigger the switch. Among the PVC thermal decomposition/combustion products, HCl and CO2,which ionization energies (12.74 eV, 13.77 eV respectively) were higher than the energy of photon (10.60 eV), were ionized by MEPEI, while alkenes, dichloroethylene, benzene and its homologs, monochlorobenzene, styrene, indane, naphthalene and its homologs were ionized by SPI and MEPEI simultaneously. Spectra of interested products as a function of temperatures indicated that products are formed via two main mechanisms: (1) dechlorination and intramolecular cyclization can lead to the formation of HCl, benzene and naphthalene at 250-370℃; (2) intermolecular crosslinking leads to the formation of alkyl aromatics such as toluene and xylene/ethylbenzene at 380-510℃. The experimental results show that the combined ion source of SPI/SPI-MEPEI for TOF-MS has broad application prospects in the online analysis field.
