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Cadmium sulfide (CdS) nanoparticles formed within Langmuir-Blodgett (LB) films of stearic acid and calixarene were studied with different optical methods including surface plasmon resonance (SPR), ellipsometry and UV-visible absorption and fluorescence spectroscopies. For the first time, the process of formation of CdS nanoparticles within LB films was monitored in-situ with SPR. The results of ellipsometry, SPR and UV-vis absorption spectroscopy were analyzed to evaluate simultaneously the thickness, refractive index and extinction coefficient of LB films. It was shown that all three parameters increase as a result of formation of CdS nanoparticles. Photoluminescence measurements provided direct confirmation directly for previous observation with UV-vis absorption spectroscopy of the blue spectral shift caused by CdS particles formation. The observed large Stoke's shift of the luminescence band is discussed in terms of the formation of "dark excitons" in the platelet-type CdS nanoclusters. AFM study shows the formation of pseudo-two dimensional platelets of CdS with the lateral dimensions in the range of 20-30 nm.