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Phase purity determination is an essential step in the characterization of solid-state materials, typically conducted through powder X-ray diffraction (XRD). However, the reparation of powder samples is often time-consuming, can lead to material wastage, and risks altering the structural properties of the sample. In this study, we present an alternative method that involves the direct use of pelletized samples for XRD analysis, bypassing the need for powdering. Our investigation, conducted on 2 series of compounds or 6 samples of oxygen-deficient perovskite oxides, demonstrates that diffraction patterns from pellet samples are sufficiently distinct to confirm phase purity, offering a faster, more efficient alternative to traditional powder XRD methods. This method not only reduces the time and effort involved in sample preparation but also preserves the material's structural and physicochemical integrity. By minimizing the mechanical manipulation and thermal exposure of the samples, the direct pellet method allows for subsequent property measurements—such as electrical conductivity, magnetic behavior, thermoelectric behavior, catalytic activity, and electrode performance—without risking sample degradation. Our results show that this approach provides reliable phase purity assessment while conserving materials, making it an attractive option for researchers working with oxygen-deficient perovskite oxides and other complex materials.