Cognitive deficits are repeatedly described with Pb exposure, but little is known about the distribution of lead in brain. To determine the local distribution of lead (Pb) and other trace elements, X-ray fluorescence spectroscopy measurements have been performed, using a microbeam setup and highest flux synchrotron radiation. Experiments have been carried out at ID-22, ESRF, Grenoble, France. The installed microprobe setup provides a monochromatic beam (16 keV) from an undulator station focused by Kirkpatrick-Baez X-ray optics to a spot size of 5 μm×3 μm. Brain slices from frontal cortex, thalamus, and hippocampus have been investigated (20 μm thickness, imbedded in paraffin and mounted on kapton foils). In general no significant increase in fluorescence intensities could be detected in one of the investigated brain compartments. Pb and other (trace) elements such as S, Ca, Fe, Cu, Zn, and Br could be detected in all samples and showed strong inhomogeneities within the analysed areas. While S, Ca, Fe, Cu, Zn, and Br could be clearly assigned to brain vessel structures (blood vessels, plexus choroidei), Pb was very inhomogeneously distributed. The local distribution of the detected elements in various brain structures will be discussed.