The application of sample rotation during SIMS analysis of practical samples is described. It is shown that sample rotation gives improved depth resolution in profiles of metal layers on flat semiconductor substrates, allowing thin interfacial layers to be identified. For thick metal layers on non-ideal substrates, the benefits of sample rotation are less clear. Sample rotation is also shown to be useful as a simple in situ sample preparation tool for the removal of metal overlayers on semiconductor substrates where the objective of the analysis is the semiconductor material rather than the metal itself, Copyright (C) 1999 John Whey & Sons, Ltd.