Direct Temperature Resolved HRMS of Fire-Retarded Polymers by In-Source PyMS on an External Ion Source Fourier Transform Ion Cyclotron Resonance Mass Spectrometer
Direct Temperature Resolved HRMS of Fire-Retarded Polymers by In-Source PyMS on an External Ion Source Fourier Transform Ion Cyclotron Resonance Mass Spectrometer
复制标题
在外部离子源傅里叶变换离子回旋共振质谱仪上通过源内 PyMS 直接温度分辨阻燃聚合物的 HRMS
DOI：
--
复制
发表时间：
1995
期刊：
影响因子：
--
通讯作者：
J. Boon
中科院分区：
文献类型：
--
作者：
R. Heeren;C. G. Koster;J. Boon
具有高质量精度的快速微尺度分析证明了直接温度分辨解吸和热解从Pt/Rh灯丝探针内部的外部离子源的7-T FTICR-MS。解吸和热解过程中产生的离子源的高压不干扰分析中的无烃超高真空的ICR细胞，从而允许在高分辨率短的观察周期。在典型条件下，m/z为600，循环时间为100 ms，质量分辨率（m/Δm）50%= 50 000，用于分析掺锑阻燃剂的溴化阻燃聚合物热解产生的同量异序化合物混合物。从家用电器中取样的不明阻燃聚合物混合物被发现含有溴化联苯、溴化二苯醚、四溴双酚A及其丁基化异构体、聚苯乙烯和氧化锑。通过源内热解FTICR-MS进行的高分辨率温度分辨分析证实了元素组成。该分离度足以将标称同量异位素离子与氧化锑（III）（Sb 4 O 6）和四溴双酚-A的正丁基醚衍生物分离。
Rapid microscale analysis with high mass accuracy is demonstrated by direct temperature resolved desorption and pyrolysis from a Pt/Rh filament probe inside the external ion source of a 7-T FTICR-MS. High pressure generated during desorption and pyrolysis in the ion source does not interfere with analysis in the hydrocarbon-free UHV of the ICR cell, thus allowing short observation cycles at high resolution. The typical conditions achieved, a mass resolution (m/Δm) 50% equals 50 000 at m/z 600 with cycle times of 100 ms, were used to analyze isobaric compound mixtures generated by pyrolysis of brominated fire-retarded polymers spiked with antimony-containing synergists. Unknown fire-retarded polymer blends sampled from household appliances were found to contain brominated biphenyls, brominated diphenyl ethers, tetra-bromoBisphenol-A and its butylated isomers, polystyrene, and antimony oxides. High-resolution temperature-resolved analysis by in-source pyrolysis FTICR-MS confirms the elemental composition. The resolution is sufficient to separate the nominally isobaric ions from the antimony(III) oxide (Sb 4 O 6 ) synergist and the n-butyl ether derivative of tetrabromoBisphenol-A.