Neutron activation analysis has been used to detect trace amounts of sodium and potassium in solid rocket propellants containing aluminum. The technique followed employs a water-pool reactor to irradiate the samples with thermal neutrons, and utilizes gamma-ray spectroscopy to nonde-structively analyze the samples for trace impurities. This technique permits precise and accurate determination of sodium and potassium in solid propellants containing as much as 20% aluminum.