X-ray diffraction (XRD), grazing incidence X-ray diffraction (GIXRD) and X-ray reflectometry (XRR) techniques were applied for analysis of titanium (Ti) and titanium (IV) oxide (TiO2) nanolayers with thickness of 25 nm, 50 nm and 75 nm deposited on silicon, quartz and BK7 glass substrates. The aim of studies was investigating the crystal structure and morphology of the nanolayers in dependence on the substrate type. The chemical phases of nanolayers and substrates were determined by using the XRD and GIXRD measurements. The benefits of applying low angle GIXRD and XRR analytical techniques, both for substrate and nanofilm analysis, is discussed based on theoretical calculations and simulations. Additional, analytical capabilities of the XRR technique to nanolayer and substrate morphology analysis are presented. Simulated XRR curves for titanium (Ti) and titanium (IV) oxide nanolayers are discussed depending on the substrate type as well as the substrate and nanolayer roughnesses. Experimental reflectometry curves are presented for all titanium and titanium (IV) oxide nanolayers deposited on the different substrates. As the result of the XRR analysis, the nanolayer thickness and roughness together with substrate roughness are estimated. The mean values of the Ti and TiO2 layer thickness and roughness are presented for all studied samples. The largest roughness, both for nanolayers and for substrates, is obtained for BK7 glass material. In the manuscript, sample properties, experimental setups and measurement conditions are presented in details.