Institute of Physical and Inorganic Chemistry, University of Bremen, FB 2, Bremen, Germany.
Research Unit Analytical BioGeoChemistry, Helmholtz Zentrum München, Neuherberg, Germany.
Mass Spectrom Rev. 2022 Mar;41(2):338-351. doi: 10.1002/mas.21682. Epub 2021 Jan 31.
The world of Fourier-transform ion cyclotron resonance (FT-ICR) mass spectrometry has witnessed, especially in the last 30 years significant advances in many fields of science, such as electronics, magnets, new ICR cell designs, developed ICR event sequences, modern external ionization sources, and linear ion beam guides, as well as modern vacuum technology. In this review, a brief account is given focusing especially on the studies performed in Wanczek's group and ICR research laboratory at the University of Bremen. An FT-ICR mass spectrometer has been developed with a high magnetic field superconducting magnet, operating at 4.7 T. At this magnetic field, a trapping time of 13.5 h was obtained with 30% efficiency. For the tetrachloromethane molecular ion, m/z 166, a mass-resolving power m/Δm = 1.5 × 10 was measured at a pressure of 2 × 10 Torr. The transition from magnet sweep to frequency sweep and the application of Fourier-transform has greatly enhanced the ICR technology. External ion sources were invented and differential pumping schemes were developed for enabling ultrahigh vacuum condition for ICR detection, while guiding ions at relatively higher pressures, during their flight to the ICR cell. With the external ion source, a time-of-flight ICR tandem instrument is built. A method to measure the ion flight time and to trap the ions in the ICR cell is described. Many ICR cell characteristics such as z-axis ion ejection and coupling of radial and axial ion motions in a superposed homogeneous magnetic and inhomogeneous trapping electric field were extensively studied. Gas-phase ion-molecule reactions of several reactive inorganic compounds with a focus on phosphorous and sulfur as well as silicon chemistry were also studied in great detail. The gas-phase ion chemistry of several trifluoromethyl-reagents such as trifluoromethyltrimethylsilane and tris(trifluoromethyl)phosphine were also investigated in ICR. Dual polarities multisegmented ICR cells were invented and deeply characterized. Sophisticated ICR pulse event programs were developed to enable long-range ion-ion interactions between simultaneously trapped positive and negative ions.
傅里叶变换离子回旋共振（FT-ICR）质谱领域在过去 30 年中见证了许多科学领域的重大进展，如电子学、磁铁、新型 ICR 单元设计、开发的 ICR 事件序列、现代外部离子源、线性离子束导向器以及现代真空技术。在这篇综述中，我们简要介绍了特别是在万采克（Wanczek）小组和不来梅大学 ICR 研究实验室的研究进展。我们开发了一台带有超导磁体的高磁场 FT-ICR 质谱仪，磁场强度为 4.7T。在该磁场下，采用 30%的效率获得了 13.5 小时的捕获时间。对于四氯甲烷分子离子 m/z 166，在 2×10 -2 Torr 的压力下，测量得到的质量分辨率 m/Δm=1.5×10。从磁场扫描到频率扫描的转变以及傅里叶变换的应用极大地增强了 ICR 技术。发明了外部离子源，并开发了差分抽气方案，以实现 ICR 检测的超高真空条件，同时在离子飞向 ICR 单元的过程中，在相对较高的压力下引导离子。采用外部离子源，构建了飞行时间 ICR 串联仪器。描述了一种测量离子飞行时间并将离子捕获在 ICR 单元中的方法。广泛研究了 ICR 单元的许多特性，如 z 轴离子喷射以及在叠加的均匀磁场和非均匀捕获电场中的径向和轴向离子运动的耦合。还详细研究了几种无机反应性化合物的气相离子-分子反应，重点是磷和硫以及硅化学。也在 ICR 中研究了几种三氟甲基试剂（如三氟甲基三甲硅烷和三（三氟甲基）膦）的气相离子化学。发明了双极性多段 ICR 单元，并对其进行了深入的特性研究。开发了复杂的 ICR 脉冲事件程序，以实现同时捕获的正离子和负离子之间的远程离子-离子相互作用。
