The quantitative phase analysis in the system Y2BaCuO5(2-1-1)-YBa2Cu3O6+x(1-2-3) was performed by the X-ray powder diffraction (XRPD) method based on the comparison of the integral intensities of the X-ray diffractions of the investigated system with the corresponding intensities of standard mixtures of (2-1-1) and (1-2-3) components of known composition. To avoid the orientation effects of the (1-2-3) components, the selected mixtures were homogenized by the admixture of 50 mass% α-AL2O3. The constituent (2-1-1) showed no preferential orientation, neither in the bulk textured materials prepared by the quench and melt growth technique, nor in the samples ground to powder. The X-ray diffraction results were in accordance with the semiquantitative estimation of the concentration of the paramagnetic (2-1-1) phase obtained from the results of EPR measurements on powdered samples. On the other hand, the intensity of the EPR spectra strongly decreased in bulk materials due to the skin effect. The electric conductivity of (1-2-3) at room temperature causes the microwave fields to penetrate to a depth of approximately 10 μm, which is the only EPR active region.