New ceramic fibers, currently in various stages of commercial development, have been consolidated in intermetallic matrices such as γ-TiAl and FeAl. Fiber types include SiC, TiB2 and polycrystalline and single crystal Al2O3. This work required the development of techniques to characterize the thermochemical stability of these fibers in different matrices.SEM/EDS elemental mapping was used for this work. To obtain qualitative compositional/spatial information, the best realistically achievable counting statistics were required. We established that 128 × 128 maps, acquired with a 20 KeV accelerating voltage, 3 sec. live time per pixel (total mapping time, 18 h) and with beam current adjusted to give 30% dead time, provided adequate image quality at a magnification of 800X. The maps were acquired, with backgrounds subtracted, using a Noran TN 5500 EDS system. The images and maps were transferred to a Macintosh and converted into TIFF files using either TIFF Maker, or TNtolMAGE, a Microsoft QuickBASIC program developed at the Science Center. From TIFF files, images and maps were opened in either NIH Image or Adobe Photoshop for processing and analysis and printed from Microsoft Powerpoint on a Kodak XL7700 dye transfer image printer.