Secondary Ion Mass Spectrometry (SIMS) can characterize the surface and near surface of Nb used in accelerator cavities. Results show Nb oxide in the 2-3 nm range, a depleted H concentration in the oxide compared with the bulk, and N, C, O lower in an annealed single crystal sample than several polycrystalline samples. Other metallic contaminants are primarily at the surface, but tantalum is distributed uniformly through the material.