The regional distribution of lithium (Li) in vivo was determined on a relative basis in the brain and muscle of rats by 7Li NMR imaging. Both high resolution 7Li NMR spectroscopy and atomic absorption spectrophotometry were performed on extracts of brain and muscle tissue from the same rats. The average in vivo results were generally in good agreement with the corresponding average in vitro results, despite the relatively low signal-to-noise ratio of the in vivo images. There was good agreement between the two in vitro methods of analysis, both on average and for individual animals. Significant differences were found in vivo among Li concentration ratios for the various brain regions and muscle by 7Li imaging, as well as by the in vitro methods.