The U.S. Bureau of Mines has developed a rapid microwave digestion technique for dissolving both gallium and germanium in solid matrices that allows for accurate analysis by flame atomic absorption spectrophotometry. Microwave digestion in sealed teflon vessels is accomplished in approximately 2 min per sample in a two- step process using hno3, hf, h3bo3, and kno3. Gallium and germanium in the produced solutions are determined with no detectable interferences using nitrous oxide-acetylene flame atomic absorption spectrophotometry. With this method, samples containing as little as 0.01 pct gallium and germanium can be accurately analyzed. Values obtained for gallium agree with certified values and neutron activation analyses. Both gallium and germanium spike recoveries approach 100 pct when taken through the digestion process. The solutions produced by this method are also suitable for analysis by electrothermal atomization.