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Ultrafast pulse radiolysis with a short-pulsed electron beam and a short-pulsed analyzing light is a powerful time-resolved spectroscopic technique to study the kinetics and reactions of short-lived intermediate species or precursors in radiation chemistry and biology. In this chapter, first, we give an overview of historical developments of ultrafast pulse radiolysis. Then, we describe a femtosecond pulse radiolysis instrument, including the generation of femtosecond electron pulses by a photocathode radio frequency (rf) gun-based linear electron accelerator, the synchronization of femtosecond analyzing laser with the electron pulses, the transient absorption measurement with double-pulse technique, and the observations of the formation processes and ultrafast reactions of hydrated electrons in water. Finally, two innovative techniques, which enable to improve the time resolution in next pulse radiolysis development, are presented.