A novel approach for the analysis of lignin in geochemical samples has been developed as an alternative to the alkaline CuO oxidation procedure first developed in 1982. The new procedure utilizes microwave digestion technology, as opposed to conductive heating, to carry out oxidative hydrolysis of six samples in an oxygen-free atmosphere at 150 degrees C for 90 min. Ethyl acetate is used as the extraction solvent in place of diethyl ether. Additionally, the new method incorporates a simplified extraction procedure that minimizes solvent handling and the amount of glassware needed. Under these novel conditions, the yields and compositions of lignin phenols from four different samples (modern and ancient sediments; woody and nonwoody tissues) match those obtained by the "traditional" procedure. The significant advantages of this new alkaline CuO oxidation method include faster reaction times, the ability to accurately measure and control reaction conditions, added flexibility for the analyst, and a marked increase in the achievable sample throughput.