A triple cell ICR spectrometer analogous to a three-stage mass spectrometer (MS/MS/MS) but capable of studying thermal energy collisions is described. The facility to store ions in a good vacuum allows the measurement of radiative lifetimes using a chemical reaction to probe the energy contents of the ions as a function of their storage time. Vibrational lifetimes have been measured for two diatomic ions in their electronic ground state: NO + and HCl +. NO + and NO have similar lifetimes, in very good agreement with calculated values. HCl + ( v = 1) has a lifetime ten times shorter than HCl (3 ± 1 ms compared with 29 ms), in fairly good agreement with the calculated value of 4.6 ms. This is the first experimental confirmation of the very short lifetimes predicted theoretically for diatomic hydride ions. Qualitative results have been obtained for the radiative lifetime of NH 3 +. The shape of the decay curves indicates the presence of long-lived (more than 300 ms) and short-lived (10–20 ms) states.