Abstract The microparticle analysis method, based on the application of a sample rotation technique in secondary ion mass spectrometry (SIMS) depth profile analysis is described. Sample rotation experiments, i.e. ion sputtering with the application of variable azimuth incidence angle of the primary beam, were performed in order to reduce a shadowing effect in the rough surface sputtering. A more uniform erosion process than in the case of standard stationary sample bombardment has been observed. The rotation technique yields a greater bombarded surface of the individual microparticles than that observed using the beam with a constant azimuth incidence angle. Surface recession induced by ion erosion of the spherical particle was modelled using the ANSYS and SRIM codes under the same conditions as those of the experimental bombardment. The results of the ion-eroded surface are shown in the case of stationary and rotating samples. Ion sputtering of microparticles was performed with 150 nA, 4 keV Ar + ion beam in the SIMS spectrometer equipped with the 16 mm QMA-410 Balzers quadrupole and the precision sample rotation manipulator. Special sample preparation methods were performed in order to obtain a mini target. Indium matrix with the attached microparticles of a known “core-shell” structure was shaped to a 0.6–0.2 mm diameter substrate.