Roentgen ray spectrometry was used to obtain element spectra from isolated samples of perilymph, endolymph, outer hair cells, and stria vascularis obtained by microdissection from the freeze-dried inner ears of chinchillas. The spectra of perilymph and endolymph residues indicated that no cross-contamination of the two cochlear fluids occurs during freeze-drying or sampling. The spectra of outer hair cells suggested that the extracellular fluid in the organ of Corti spaces is similar to perilymph in its ionic content. The spectra of stria vascularis samples indicated low sodium and high phosphorus contents. Energy-dispersive roentgen ray analysis of freeze-dried inner ears appears to be a promising method for low-contamination measurement of ion distribution in the cochlea.