A round-robin characterization is reported on the sputter depth profiling of [60×(3.0nm Mo/0.3nm B 4 C/3.7nm Si)] and [60×(3.5nm Mo/3.5nm Si)] stacks deposited on Si(111). Two different commercial secondary ion mass spectrometers with time-of-flight and magnetic-sector analyzers, a pulsed radio frequency glow discharge optical emission spectrometer, and a home-built time-of-flight low-energy ion scattering and quadrupole-based secondary ion mass spectrometer were used. The influence of the experimental conditions, especially the type and energy of sputter ions, on the depth profiles of Mo/Si nanostructures with and without B 4 C barrier layers is discussed in terms of depth resolution, modulation factor and rapidity of analysis. The pros and cons of each instrumental approach are summarized.