The optical methods to determine refractive index profile of layered materials are commonly used with spectroscopic ellipsometry or transmittance/reflectance spectrometry. Measurements of spectral reflection and transmission usually permit to characterize optical materials and determine their refractive index. However, it is possible to characterize of samples with dopants, impurities as well as defects using optical methods. Microstructures of a hydrogenated crystalline Si wafer and a layer of SiO 2 -ZrO 2 composition are investigated. The first sample is a Si (001):H Czochralski grown single crystalline wafer with 50 nm thick surface Si0 2 layer. Hydrogen dose implantation (D ≤ 4x10 l6 cm -2 ) results in a creation of porous (spongy) -like buried Si layer. Interaction between hydrogen atoms and a semiconductor, involving adsorption, surface diffusion, and desorption, continue to be an important issue in microelectronic device and sensor fabrication. Hydrogen-implanted silicon (Si: H) has become a topic of remarkable interest, mostly because of the potential of implantation-induced platelets and micro-cavities for the creation of gettering active areas and for Si layer splitting. Oxygen precipitation and atmospheric impurity are analysed. The second sample is the layer of co-evaporated SiO 2 and ZrO 2 materials using simultaneously two electron beam guns in reactive evaporation methods. The composition structure was investigated by X-Ray photoelectron spectroscopy (XPS), and spectroscopic ellipsometry methods. A non-uniformity and composition of layer are analysed using average density method.