The method for determination of N,N-dimethylhydro-xylamine(DMHAN) in water and nitric acid by capillary gas chromatography was studied in this paper.The test results showed that the linearity between the peak area and concentration was excellent in the range of 3.0×10-4~2.5×10-3 mol/L with a correlation coefficient of over 0.999.The relative standard deviation(RSD) was lower than 1.0%.The minimum detectable limit(MDL) of DMHAN was 3.0×10-4 mol/L.The possible impurities(such as methanol,formaldehyde,methanoic acid,nitric acid,monomethyl hydrazine,ethanol,hydrazine,and methylamine) did not affect the quantitative determination of DMHAN by the analytical system.