We describe a new methodology to collect energy domain Mössbauer spectra of inclusions in natural diamonds using a Synchrotron Mössbauer Source (SMS). Measurements were carried out at the Nuclear Resonance beamline ID18 at the European Synchrotron Radiation Facility (Grenoble, France). We applied this non-destructive approach to collect SMS spectra of a ferropericlase inclusion still contained within its diamond host from Juina (Brazil). The high spatial resolution of the measurement (~ 15 μm) enabled multiple regions of the 190 × 105 μm2
inclusion to be sampled and showed that while Fe3 +
values in ferropericlase were below the detection limit (0.02) overall, there was a magnetic component whose abundance varied systematically across the inclusion. Hyperfine parameters of the magnetic component are consistent with magnesioferrite, and the absence of superparamagnetism allows the minimum particle size to be estimated as ~ 30 nm. Bulk Fe3 +
values are similar to those reported for other ferropericlase inclusions from Juina, and their variation across the inclusion can provide constraints on its history.