The stable isotopic compositions of nitrogen and carbon in cyanide compounds can be determined by combusting aliquots in sealed tubes to form N 2 gas and CO 2 gas and analyzing the gases by mass spectrometry. Free cyanide (CNaq + HCN aq ) in simple solutions can also be analyzed by first precipitating the cyanide as copper(II) ferrocyanide and then combusting the precipitate. Reproducibility is (0.5‰ or better for both δ 15 N and δ 13 C. If empirical corrections are made on the basis of carbon yields, the reproducibility of δ 13 C can be improved to (0.2‰. The analytical methods described herein are sufficiently accurate and precise to apply stable isotope techniques to problems of cyanide degradation in natural waters and industrial process solutions.