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Selenium can be determined quantitatively in biological samples after digestion using nitric acid, orthophosphoric acid, and hydrogen peroxide and the formation of 5-nitropiazselenol. Samples are spiked with enriched 82Se and lsotoplc ratio of 80Se to 82Se is measured by combined gas chromatographymass spectrometry using dual ion monitoring. Precise determination at the parts-per-billion level is possible. The accuracy of the method Is verlfied by using standard reference materials.