Chem805 Identification of organic and inorganic compounds by chem805有机和无机化合物的鉴定.ppt

Fast Atom Bombardment (FAB) The sample is dissolved in a liquid matrix such as glycerol, thioglycerol, m-nitrobenzyl alcohol, or diethanolamine and a small amount (about 1 microliter) is placed on a target. The target is bombarded with a fast atom beam (for example, 6 keV xenon atoms) that desorb molecular-like ions and fragments from the analyte. Cluster ions from the liquid matrix are also desorbed and produce a chemical background that varies with the matrix used. Xe e- Xe+? + Xe Xe+? Is accelerated to ~6-10 keV, and pass through Xe Xe + Xe+? Xe (Xenon with Kinetic energy) FAB * FAB: Benefits Sample introduction can be through direct insertion probe or LC/MS (continuous-flow FAB). Benefits rapid, simple relatively tolerant of variations in sampling good for a large variety of compounds Useful fragentation pattern strong ion currents -- good for high-resolution measurements * FAB: Limitations Limitations high chemical background defines detection limits may be difficult to distinguish low-molecular-weight compounds from chemical background analyte must be soluble in the liquid matrix no good for multiply charged compounds with more than 2 charges requires a high concentration of the organic liquid matrix (typically 80 to 95% glycerol) which limits sensitivity Mass range Moderate Typically ~300 Da to about 6000 Da. * Comparing different techniques * Classification according to method of separating charged particule Magnetic Field Deflection Magnetic Field only: Mass 12-500 in seconds Double Focussing: High resolution to 4 decimalsr = 60,000  Quadrupole Mass Spectrometer Quadrupole Mass Filter: Mass Scanning by varying RF DC Frequencies Quadrupole Ion Storage (Ion Trap)- Compact-Inexpensive-Very Sensitive-GC/MS * Classification according to method of separating charged particule Time of Flight- Need Fast Electronic (10-7 s)- Used With Sophisticated Ionization Methods (FAB, Laser Desorption ….) FT-ICR (Fourier