A single-chip multichannel surface plasmon resonance sensor (SPR) has been used to detect metal ions in aqueous solutions. The equipment was designed around a commercial light-emitting diode and a CCD camera and incorporated no moving parts. The sensing materials were based on molecular architectures of polyelectrolyte films, deposited by the layer-by-layer self-assembly technique. Two bilayer architectures, poly(ethyleneimine) (PEI)/poly(ethylene-alt-maleic acid) and PEI/poly(styrenesulfonate), were shown to produce different responses to solutions containing copper, nickel, and iron. The SPR equipment was able to measure concentrations of these metals down to levels of at least 2x10-5 M.