Abstract-A rare three-phase symplectite consisting of Ca-rich pyroxene, Fe-rich olivine, and a silica phase is frequently found rimming pyroxene in the Martian meteorite Los Angeles. This assemblage is usually interpreted as the breakdown product of metastable pyroxferroite, a very rare pyroxenoid mineral itself. However, its origin is not entirely understood, mainly because the extremely small average size of the constituent phases represents a challenge for precise high-resolution analysis. In addition to electron microbeam methods, the present study uses time-of-flight secondary ion mass spectrometry (ToF-SIMS) to overcome the limits of spatial resolution and to comprehensively study this mineral assemblage. The prevailing breakdown hypothesis is supported by the following results:(1) The three symplectite phases are very homogenous in composition from 100 µm down to the micrometer scale. (2) The silica phase could be shown to be almost pure SiO 2 . (3) The symplectite bulk composition is consistent with pyroxferroite. Sub-micrometer sized Ti-oxide grains are found within the symplectite (but not within the Ca-rich pyroxene) and probably represent a minor breakdown phase in addition to the three main phases.