The X-ray diffractometer in the laboratory is a crucial instrument for analyzing materials in science. It can be used on almost any crystal material, and if the machine parameters are appropriately controlled, it can offer a lot of information about the sample’s characteristics. Nevertheless, the data obtained from these machines are complicated by an aberration function that can be resolved through calibration. In this study, a powder comprising of Barium Sulfate (BaSO4), Zinc Oxide (ZnO) and Aluminum (Al) was used as the first sample and a single crystal sample comprised of Gallium Nitride (GaN) and Aluminum Oxide (Al2O3). The required calibration parameters of the X-ray diffractometer namely: Straight Beam Alignment, Beam Cut Alignment and Sample Tilt Alignment for two samples were analyzed and carried out. Using the results of the X-ray spectrum, important parameters such as corresponding planes for peak positions, d-spacing of planes, intensities, smallest crystallite sizes and lattice parameters, and a comparison with the reference data were all carried out. As another result, the out-of-plane alignment and Full-Width- at Half-Maximum (FWHM) value for GaN could be determined using the rocking curve.