The surface of highly monodisperse magnetic iron oxide (
![](/images/gifchars/gamma.gif)
-Fe
2O
3) nanocrystals was thoroughlyinvestigated by FTIR, NMR, and mass spectroscopy. The nanocrystals were prepared by a thermaldecomposition method now widely used for the preparation of magnetic metal and metal oxide nanocrystals.This method takes advantage of oleic acid as a means to passivate the surface and render the particlesstable with respect to aggregation or grain growth and keeps them highly dispersed in a variety of organicmedia. The nature of this surface in terms of ligand structure and the role of oleic acid during the synthesisremained somewhat undetermined until this report. We provide spectroscopic evidence of an oleic acidligand structural change during
![](/images/gifchars/gamma.gif)
-Fe
2O
3 nanocrystal synthesis.