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Proper sample preparation is crucial in getting highly quality X-ray diffractometer data. If the sample has not been putted within the parameters to properly prepare XRD sample then it introduces errors that make phase identification difficult to impossible and estimates of abundances and crystallinity erroneous. Ideally, we might prefer to lead three conditions so as to own good data: (a) Total randomness of crystallite orientation. (b) Sufficient number of crystallites to induce a representative intensity distribution for the sample. (c) Sufficient diffraction intensity to satisfy counting statistics. This paper highlights the methods of perfect XRD sample preparation of solids, liquids and gases. The structurally changed materials in response to solid-gas interaction possesses great importance in many areas. The X-ray structures of liquid sodium, potassium and sodium-potassium alloys are investigated by an improved method. By employing a reservoir technique a plane surface of liquid metal has been examined by a monochromatic X-ray beam in an exceedingly focusing diffractometer.