X-Ray Diffraction.ppt

X-Ray Diffraction The XRD Technique Takes a sample of the material and places a powdered sample which is then illuminated with x-rays of a fixed wave-length. The intensity of the reflected radiation is recorded using a goniometer. The data is analyzed for the reflection angle to calculate the inter-atomic spacing. The intensity is measured to discriminate the various D spacing and the results are compared to known data to identify possible matches. Powdering Samples The samples are powdered to give a random sampling of ALL atomic planes (crystal faces) Statistically accurate given samples are powdered finely AND randomly oriented on sample holder Intensities are a reflection of d-spacing abundance Problems arise with minerals that may preferentially orient on sample holder Micas and clays have special preparation techniques X-Rays What is X-Ray Diffraction?? Crystalline substances (e.g. minerals) consist of parallel rows of atoms separated by a ‘unique’ distance Simple Example: Halite (Na and Cl) Crystalline substances (e.g. minerals) consist of parallel rows of atoms separated by a ‘unique’ distance Diffraction occurs when radiation enters a crystalline substance and is scattered Direction and intensity of diffraction depends on orientation of crystal lattice with radiation Schematic X-Ray Diffractometer Sample XRD Pattern Determine D-Spacing from XRD patterns Bragg’s Law nλ = 2dsinθ n = reflection order (1,2,3,4,etc…) λ = radiation wavelength (1.54 angstroms) d = spacing between planes of atoms (angstroms) θ = angle of incidence (degrees) Factors that affect XRD data Sample not powdered fine enough May not give all d-spacing data (not random enough) Analysis too fast (degrees/minute) May not give accurate peak data Mixture of minerals?? Not crystalline – glass!! Mixture of 2 Minerals Applications of XRD Unknown mineral ID Solid solution ID (e.g. feldspars, olivine) Mixtures of minerals Clay analyses Zeolites Crystallographic applications Material Science *