Secondary ion mass spectrometry (SIMS) has been used to guide the search fo
r an oxidation procedure that can produce a thin and relatively sharp oxide
layer on macroscopic zirconium. A new preparation based on dip coating in
H2O2 solution is indicated to be suitable for this purpose. SIMS further in
dicates that the oxide interface, for such a prepared sample, shows substan
tial degradation when it is heated in H-2 gas at 300 degrees C. The presenc
e of H appears to facilitate O migration into the metallic region, an obser
vation that supplements those made previously on oxidized thin-film samples
of zirconium prepared by deposition under ultrahigh-vacuum conditions.