This study demonstrates the possibility of a reversible naked-eye detection method for submicromolar levels of cadmium(II) using the Langmuir-Blodgett (L-B) technique. Molecular assemblies of 4-n-dodecyl-6-(2-thiazolylazo) resorcinol are transferred on precleaned microscopic glass slides, to act as a sensing probe. Isotherm (π-A) measurements were performed to ensure the films' structural rigidity and homogeneity during sensor fabrication. The sensor surface morphology was characterized using atomic force microscopy and scanning electron microscopy. The probe membrane exhibits visual color transition, forming a series of reddish-orange to pinkish-purple complexes with cadmium, over a wide concentration range (0.04-44.5 μM). Cadmium response kinetics and the changes in the sensors' intrinsic optical properties were monitored using absorption spectroscopy and further confirmed using X-ray photoelectron spectroscopy. A hybrid L-B film composite of poly(vinyl stearate) and pory(vinyl-N-octadecylcarbamate) were investigated for enhancing sensor performance. The sensor was tested for its practical approach to prove its cadmium selectivity and sensitivity amid common matrix constituents using synthetic mixtures and real water samples. Using the sensor strips, the respective lower limits of cadmium detection and quantification are 0.039 and 0.050 μM, as estimated from a normalized linear calibration plot. © 2007 American Chemical Society.