Abstract: A procedure for monitoring alkaline delignification, in particular kraft cooking, of wood or other cellulosic material with the aid of the mutually relative concentrations of the monomeric lignin hydration products which are formed in connection therewith and are dissolved in the spent liquor. According to the procedure, a sufficient number of representative spent liquor samples is taken during the cooking process which are analyzed by gas chromatography. On the basis of the concentration proportions of certain compounds which have been analyzed, that time period is determined in each instance which is required to reach the desired degree of delignification.