A system made up by a Zymark robot and a separation automate preteats spent fuel samples and monitors a tri-n-octylphosphine oxide column extraction chromatographic procedure in order to isolate and purify uranium and plutonium present in the samples, prior to the spectrometric measurements. Up to 16 subsamples of spent fuel in dried or solution form are handled simultaneously in a completely unattended mode. The throughput of the robotized analytical procedure has increased by a factor of 3 compared to the earlier manual procedure without loss in the quality of the chemical treatment and of the mass- and α-spectrometric measurements.