Thin films of plasma polymer were prepared from unsaturated precursor with one triple bond, iso-t-pentinol. This precursor was injected either in a vapor state itself or using argon as a carrier gas, bubbled through a precursor. These polymers were prepared under different fixed conditions when only one parameter of plasma polymerization among all the others was changed in each measurement during the process of polymerization (i.e., power in a matched reactor, precursor partial pressure, total pressure in reactor, electrode gap, and polymerization time). The samples were deposited on thin solid substrate having oxygenless molecules. Infrared Spectroscopy, IRS, Electron Spectroscopy for Chemical Analysis, ESCA (XPS), and Electron Paramagnetic Resonance (EPR) were used for analyses of these samples. The results of analyses proved generation and growth of oxygen-containing groups by plasma polymerization (IRS); they also proved that C-O- group concentration increased and C=O group concentration decreased in polymer surface layers during 24 h after plasma polymerization (ESCA). A drop of free radical concentration (measured by EPR) was steep from the end of plasma polymerization to 60 min and mild later on (to approximately 215 h). Amount of free radicals depended on the power in reactor.