We describe the design and current performance of a 14.5 T hybrid linear quadrupole ion trap Fourier transform ion cyclotron resonance mass spectrometer. Ion masses are routinely determined at 4-fold better mass accuracy and 2-fold higher resolving power than similar 7 T systems at the same scan rate. The combination of high magnetic field and strict control of the number of trapped ions results in external calibration broadband mass accuracy typically less than 300 ppb rms, and a resolving power of 200,000 (m/Delta m50% at m/z 400) is achieved at greater than 1 mass spectrum per second. Novel ion storage optics and methodology increase the maximum number of ions that can be delivered to the FTICR cell, thereby improving dynamic range for tandem mass spectrometry and complex mixture applications.
Products of the reaction of C(60) with H(2) gas have been monitored by high-resolution atmospheric pressure photoionization Fourier transform ion cyclotron resonance mass spectrometry (APPI FT-ICR MS), X-ray diffraction, and IR spectroscopy as a function of hydrogenation period. Samples were synthesized at 673 K and 120 bar hydrogen pressure for hydrogenation periods between 300 and 5000 min, resulting in the formation of hydrofullerene mixtures with hydrogen content ranging from 1.6 to 5.3 wt %. Highly reduced C(60)H(x) (x > 36-40) and products of their fragmentation were identified in these samples by APPI FT-ICR MS. A sharp change in structure was observed for samples with at least 5.0 wt % of hydrogen. Low-mass (300-500 Da) hydrogenation products not observed by prior field desorption (FD) FT-ICR MS were detected by APPI FT-ICR MS and their elemental compositions obtained for the first time. Synthetic and analytical fragmentation pathways are discussed.
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