This paper presents an experimental study of electron and negative ion dynamics in a pulsed 100 MHz capacitive discharge. The plasma is produced in an O 2 and Ar/O 2 /C 4 F 8 gas mixture at 2 Pa gas pressure. Laser photo-detachment combined with a microwave resonance probe is used to diagnose the absolute densities of multiple negative ion species, F − and O − . In pure oxygen discharge, both the quasi-steady state electron and negative ion densities increase during the active glow with an increase in RF power level. In the afterglow plasma, the electron density decay rate is ∼10-15 μs, whereas the O − decays more slowly with a decay time constant in the range of 30-35 μs. At a low RF power, a peak in the O − density is observed in the early afterglow plasma. In the Ar/O 2 /C 4 F 8 gas mixture, the quasi-steady state electron density in the active glow plasma increases with RF power, whereas the O − density decreases and F − density increases. In comparison to pure O 2 discharge, in the Ar/O 2 /C 4 F 8 gas mixture the electron density decay is faster. In the afterglow the F − density is ten times higher than the O − density. These results suggest a change in the dominant negative ion production mechanism within the discharge pulse from dissociative electron attachment of C x F y in the active on-phase to electron attachment to fluorine atoms in the afterglow plasma.