A double-layer chemo-chip for the characterization of liquid analytes by rapid fluorimetric imaging is described. The chemo-chip consists of an array of polymeric micro-spots prepared on a glass slide. Each spot is composed of a thin indicator layer made of PVA doped with an immobilized fluorescence dye and a top layer polymer spot with different permeation properties. The analytes can be differentiated by variations in the optical response rate of the indicator dye after its application. Consequently, different cross-linker concentrations were applied using the Nano-Plotter((TM)) which formed top layers of varying permeability. The chemo-chips were tested with the aqueous solutions of two model liquids (aqueous solutions of malonic acid and phenanthroline hydrochloride). It was found that the transition time of response had changed considerably (up to a factor of about 10) depending on different local cross linking degrees. This has resulted in time-dependent fluorescent patterns of the fluorescence images of the micro-array. The response was fast and the transition times were in the range between a few seconds to 30 s.