CdS nanoparticles were prepared and simultaneously loaded on the ion exchange resin microspheres via a simple in-situ gas-solid reaction. X-ray diffraction (XRD), scanning electron microscope (SEM), EDX analysis and UV-vis spectra were used to characterize the products. The results indicated that the CdS nanoparticles were loaded on the ion exchange resin microspheres, and the average size of particles was approximately 5.3 nm. The nanoparticle coverage was high so that a continuous nanoparticle shell formed on the ion exchange resin microspheres. In addition, the effect of Pb2+ ions (aq.) on the luminescence of the CdS nanoparticles immobilized on the ion exchange resin microspheres were investigated. It was found that the luminescence intensity of the CdS nanoparticles changed significantly when Pb2+ ions were adsorbed on the sample. The lowest concentration of Pb2+ ions that can make the intensity change is 1.0´10-20 mol×dm-3, which implies that the CdS nanoparticles immobilized on the ion exchange resin microspheres are very sensitive to Pb2+ ions (aq.).