Nitric oxide (NO) is a gaseous diatomic molecule that is biosynthesized in mammals, and it regulates a host of physiological processes including blood pressure. Over the last several years, there has been an increased interest in the redox partner HNO and its identifiable dimerization product N 2 O. This latter gaseous species is also the product of various NO-coupling reactions as occurs in bacterial NO-detoxification processes. An attractive new tool will be the ability to simultaneously detect NO and N 2 O from the same reaction vessel. We demonstrate proof-of-concept methodology for such a simultaneous and specific NO and N 2 O detection from the same precursor (from Angeli's salt decomposition) using tunable diode laser absorption spectroscopy without the need for separation or pretreatment of these gases.