The present invention provides a means of producing nitric oxide (NO) by photolysis of nitrous oxide (N2O) at ultraviolet wavelengths. One application is the production of a known concentration of NO in a diluent gas for calibration of analytical instruments that measure nitric oxide in gases such as exhaled breath, ambient air and automobile exhaust. A potentially important medical application is the production of NO for inhalation therapy, an advantage being that very little toxic NO2 gas is produced. The method is useful for producing NO for industrial applications as well. Advantages of this method of NO production include the use of a single, inexpensive, readily available reagent gas of very low toxicity. Furthermore, the concentration of NO produced can be easily controlled by varying the ultraviolet (UV) lamp intensity and relative gas flow rates. The method may also be applied to the production of controlled concentrations of other gases as well such as CO and F2 by using reagent gases other than N2O.