Among various semiconductor compounds, the nanocrystals belonging to II-VI groups were the most studied since they exhibit interesting size-tunable optical properties due to the strong quantum confinement effect. To synthesis ZnS nanoparticles by HTSPS metod, the following materials were used: zinc acetate dehydrate, diphenyl ether, oleic acid as a surfactant, sulfur powder, tributylphosphine. The reaction mixture was maintained for 2 hours at 1500C. The FTIR analysis of ZnS nanoparticles show that the peaks appearing at 1094,09 cm-1 are due to Zn-S vibration and peaks at 2920.6 cm-1 are due to microstructure formation of the samples [1]. The absorption peaks at 2850 cm-1 correspond to the stretching vibrations of –CH2−. While the peaks at 1398.57 and 896 cm-1 correspond to the bending vibration of C−O [2]. For an alltrans alkyl-chain, as in the case of crystalline n-alkanes, the symmetric and antisymmetric stretching frequencies are in the range 2846-2850 and 2916-2920 cm-1, respectively. At room temperature, the positions of the symmetric νsym(CH2) mode, 2850 cm-1, respectively are characteristic of conformationally ordered alkyl chains [3]. The bands at 722.0 cm-1 and 743.7 cm-1 are assigned to the rocking of CH2 band, which is an indicative of a long chain linear aliphatic structure and is attributes to a crystallinity and a high degree of regularity for the linear backbone structure [4]. The spectral pattern of the progressive bands reflects very sensitively the stem length of the zigzag chain. The observed progressive infrared bands in the region 720-1000 cm-1 are due to the CH2 rockingtwisting and the band observed in the region 1199.98-1398.57 due to CH2 wagging. The infrared CH2 rocking [ρ(CH2)] − 722 cm-1 and CH2 scissoring [δ(CH)] − 1460 cm-1 bands split into a doublet [5]. The principal distinction between the IR speactra of free oleic acid and coated nanoparticles consists of a disappearance of the sharp peak at 1710 cm-1 relating to the C=O stretching mode and growth of two new bands corresponding to the asymmetric νas(COO-) stretch 1525-1560 cm- and the symmetric νs(COO-) stretch at 1400 cm- due to C=O bond rupture. These facts also the absence of the free oleic acid and permit us to assume that the nanoparticles is surrounded with relatively close-packed organic monolayer [4].