The X-ray diffraction is a useful tool for research work and different types of analysis like powder analysis, texture analysis, stress analysis, single crystal analysis, high-resolution analysis. All of these studies are under nondestructive testing.This book emphasizes on structure determination techniques of transition metal chalcogenides using x-rays diffraction. Work presented in book mainly describes the use of Powder X-ray Diffraction (PXRD) and single crystal diffraction calculations for the determination of crystal structure for transition metal chalcogenides.