The deposition of alternating layers of pectin and chitosan at a solid surface was studied using surface plasmon resonance. The binding of biopolymer to the surface was irreversible over the time scales examined. The deposition was dependent on the flow rate through the measurement cell with mass transport limitation at lower flow rates. The thickness of the deposited layer was dependent on the biopolymer concentration and was particularly marked for pectin. This was consistent with a process of initial attachment, followed by a slower structural rearrangement, which was inhibited at high initial surface concentrations of adsorbed biopolymer. Sequential deposition resulted in the formation of multilayers with an essentially linear growth rate.