Monitoring of volatile fatty acids (VFA) by gas chromatography or hydrogen with specific electrodes is used for the determination of instability in anaerobic reactors. However, such methods are not normally applied in full-scale reactors due to the need for expensive equipment. A two end-point alkalimetric method has been proposed in the literature for the follow-up and control of anaerobic digesters. This paper deals with results of the start-up and operation of a laboratory UASB (Upflow Anaerobic Sludge Blanket) reactor (5.61) treating potato-starch wastewater, where such an alkalimetric method was simultaneously used and compared with gas-chromatography VFA monitoring.