A method has been developed for the determination of ppb levels of U contents in reactor materials by neutron activation analysis. The method was applied to the determination of U in various materials, most of which are used in the JMTR (Japan Materials Testing Reactor). The sample specimens were irradiated in a nuclear reactor, together with U standard solutions. For Zircaloy, stainless steel, Al and demineralized water, analyses were carried out by measuring the γ-ray spectra of 239Np after being separated by TTA-xylene liquid-liquid extraction method. However the analyses of graphite and Be samples were carried out without the chemical separation. The analytical results were as follows, Zircaloy: 40-200ppb, stainless steel: less than 40ppb, graphite: less than 0.4ppb, demineralized water for JMTR: less than 0.5ppb, Al: 200-300ppb, Be: 10-40ppm. Agreements were satisfactory between the present results and the certified values in reference materials of Zircaloy.