In an endeavor to facilitate the use of stable isotopes in biological tracer research, we have developed a simple, real time procedure for reasonably accurate optical emission analysis of <sup>15</sup>N and <sup>13</sup>C in ammonium salts and bicarbonates, respectively. The amount of sample required for each analysis is in the range 10 to 100 μmol. In the procedure proposed, complicated chemical techniques have been avoided through (1) decomposition of the sample by heating; (2) removal of unwanted compounds, and regulation of pressure, by cooling; and (3) production of N<sub>2</sub> and CO<sup>+</sup> from NH<sub>3</sub> and CO<sub>2</sub>, respectively, by electrodeless microwave interaction. These three steps are followed by (4) measurement of relevant peak heights in the N<sub>2</sub> and CO<sup>+</sup> spectra obtained.
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