Based on the absorption property of glyoxime which can be formed by addition reaction of aldehyde group and hydroxylamine in the UV-spectral region,spectrophotometric determination of glyoxal in glyoxal solution was proposed.Linearity for the determination of glyoxal was found in the ranges of 8.4×10-6~7.2×10-5 mol/L and its regression equation was obtained.The mean recovery for glyoxal is 101.1%(n=8) and RSD is 0.75%.The method can be used for the analysis of glyoxal in the oxidation of acetaldehyde by nitric acid.