Glucose was separated ft-om fructose experimentally using a simulated moving-bed (SAM adsorber. A strongly, acid cationic resin of gel type (Ca2+ form) Dowex Monosphere (d(p) - 320 mum) was used in a pilot SMB unit of twelve 26 X 300 min (ID X length) columns. A recently proposed design procedure was applied to overcome the inherent strong mass-transfer resistance present in this kind of adsorbent. The fluid/solid velocity ratios in SMB sections 1, 2 and 3 leading to at least 90% product purity were followed by simulation and plotted in a 3-D parameter space. The design methodology, called "separation volume analysis, "also considered the geometric parameters, as well as allowable working flow rates, temperature and pressure of the plant. Operating conditions from this procedure were used to operate the SMB unit, and the expected performance was achieved experimentally Simulation strategies based on a true counter-current and a real SMB were used and the predicted performance of both agreed well with experimental data. Furthermore, experimental results confirmed predictions of the separation volume analysis, which shows the potential of the technique for optimizing existing SMB equipment.