Sample decomposition method with alkaline CuO oxidation procedure in determination of lignin in sediment samples, firstly developed by Hedges and Ertel, has been improved. Sediment samples were decomposed with oxidative-alkaline CuO in a microwave-assisted digestion system and then lignin monomers were determined by gas chromatography. The factors affecting the oxidative decomposition efficiency of the lignin were investigated. The results indicated that the best decomposition condition was 150 ℃ for 90 minuend the optimized condition, recovery for lignin monomers was 91.4%~108% with average precision of 4.5% RSD.