A sampled delayed scheme is proposed to regulate the organic pollution level in anaerobic digestion processes by using off-line COD measurements. The proposed scheme is obtained by combining an error feedback control with a steady state estimator to track constant references and attenuate process load disturbances. The controller performance is tested experimentally for the treatment of tequila vinasses over a period of 68 days under different set-point values and several uncertain scenarios which include badly known kinetic parameters and load disturbances. Experimental results show that the COD concentration can be effectively regulated under the influence of set-point changes and high load disturbances by using only a daily off-line COD measurement, which makes the industrial application of the proposed control scheme feasible. (C) 2011 Elsevier Ltd. All rights reserved.